Systems for custom coloration
Abstract
A set of a device for the preparation of a personalized composition for the treatment of hair and an optical measuring instrument for the evaluation of the initial properties of said hair, the composition comprising a plurality of solid formulations that are in tablet form, comprising the device - a plurality of containers, each container having - an outlet suitable for supplying a solid formulation which is in tablet form; and - a dispenser unit for supplying a predetermined quantity of tablets, said containers and said dispenser unit being able to connect to each other, - at least one computer-implemented unit, the computer-implemented unit being interconnected with said dispensing unit for each of said containers , the computer-implemented unit selecting the predetermined quantity of tablets distributed by said dispensing unit of each of said containers after evaluation of the initial properties of said hair carried out by means of the optical measuring instrument.

Term
5.5 yearsto projected expiry
Projected expiry 21 March 2032, counted from filing; an application has no term until it is granted.
- Priority
- Filed
- Published
- Today
- Projected expiry
12 claims: 8 independent, 4 dependent
- 1ES 2 823 977 T3 REIVINDICACIONES 1. Un conjunto de un dispositivo para la preparación de una composición personalizada para el tratamiento del cabello y un instrumento de medición óptica para la evaluación de las propiedades iniciales de dicho cabello, comprendiendo la composición una pluralidad de formulaciones sólidas que están en forma de comprimido, comprendiendo el dispositivo - una pluralidad de recipientes, teniendo cada recipiente • una salida adecuada para suministrar una formulación sólida que está en forma de comprimido;y • una unidad distribuidora para suministrar una cantidad predeterminada de comprimidos, pudiéndose conectar dichos recipientes y dicha unidad distribuidora entre sí, - al menos una unidad implementada por ordenador, estando la unidad implementada por ordenador interconectada con dicha unidad distribuidora de cada uno de dichos recipientes, seleccionando la unidad implementada por ordenador la cantidad predeterminada de comprimidos distribuidos mediante dicha unidad distribuidora de cada uno de dichos recipientes tras la evaluación de las propiedades iniciales de dicho cabello efectuada mediante el instrumento de medición óptica.
- 2El conjunto de la reivindicación 1, en donde cada uno de dichos recipientes comprende, individualmente, un tipo diferente de comprimidos, en donde dicha composición de tratamiento personalizada comprende dicha cantidad predeterminada de cada uno de dicho al menos un tipo de dichos comprimidos, en donde dicha composición personalizada comprende una combinación de al menos dos tipos diferentes de comprimidos, suministrándose cada uno de dichos tipos de comprimidos a partir de un recipiente diferente, en donde al menos un tipo de dichos tipos de comprimidos comprende un agente que confiere coloración.
- 3El conjunto de la reivindicación 2, en donde al menos un tipo de dichos tipos de comprimidos comprende comprimidos de disgregación rápida.
- 4El conjunto de cualquiera de las reivindicaciones 1 a 3, en donde el tiempo de disgregación de cada una de las formulaciones sólidas en agua desionizada es no mayor de 2 minutos.
- 5El conjunto de cualquiera de las reivindicaciones 2 a 4, en donde al menos una de dichas formulaciones sólidas comprende al menos un superdisgregante insoluble en agua y al menos un agente activo seleccionado del grupo que consiste en un agente que confiere color, un agente alcalinizante, un agente oxidante y un agente espesante, estando dicho superdisgregante caracterizado por una proporción de absorción de agua de al menos 0,5, estando la proporción de absorción de agua definida como el cambio en el peso después de la humectación del comprimido dividido por el peso del comprimido seco.
- 6El conjunto de la reivindicación 5, en donde dicho superdisgregante es un polímero reticulado.
- 7El conjunto de la reivindicación 4 o 5, en donde dicho al menos un agente activo consiste en dicho al menos un agente que confiere color seleccionado del grupo que consiste en un precursor de tinte, un acoplador de tinte, un tinte directo y cualquier combinación de los mismos.
- 8El conjunto de cualquiera de las reivindicaciones 1 a 7, que comprende, además, al menos un embudo configurado para encauzar los comprimidos distribuidos a partir de dicho recipiente hasta una salida.
- 9El conjunto de acuerdo con cualquiera de las reivindicaciones 1 a 8, en donde dicha composición personalizada comprende una combinación de al menos dos tipos diferentes de comprimidos, estando cada uno de dichos tipos de comprimidos distribuidos a partir de un recipiente diferente, en donde al menos un tipo de dichos tipos de comprimidos comprende un agente que confiere coloración, en donde al menos un tipo de dichos tipos de comprimidos comprende un agente activo seleccionado del grupo que consiste en un agente oxidante, un agente alcalinizante y un agente espesante, estando el dispositivo configurado para generar al menos un medio seleccionado del grupo que consiste en un medio alcalinizante, un medio blanqueante, un medio oxidante y un medio espesante, comprendiendo al menos un compartimento adicional que contiene al menos uno de los medios y estando configurado para suministrar cada uno de al menos un medio en una cantidad predeterminada.
- 10El conjunto de acuerdo con cualquiera de las reivindicaciones 1 a 9, el instrumento de medición óptica y el medio implementado por ordenador están diseñados de tal manera que se realiza la determinación de los componentes y sus concentraciones en la composición al tiempo que se evalúan las características químicas y físicas del cabello a tratar y el resultado deseado a lograr para proporcionar, por tanto, un tratamiento personalizado.
- 11El conjunto de acuerdo con cualquiera de las reivindicaciones 1 a 10, en donde dicho instrumento de medición 110 ES 2 823 977 T3 óptica comprende:una unidad de iluminación para iluminar el cabello;una unidad de medición que comprende al menos un sensor para la medición óptica de dicho cabello durante la iluminación mediante dicha unidad de iluminación;en donde el sensor y un haz de la unidad de iluminación, respectivamente, usan longitudes de onda en las regiones espectrales visible e infrarroja, para proporcionar, de ese modo, un espectro de dicho cabello que distingue tanto entre diferentes colorantes de cabellos naturales como entre diferentes colorantes de cabellos artificiales.
- 12Un método de realización de un tratamiento personalizado del cabello con el conjunto de acuerdo con cualquiera de las reivindicaciones 1 a 11, comprendiendo el método:obtener mediciones ópticas del cabello;predecir el resultado del tratamiento del cabello con una combinación predeterminada de agentes activos, al tiempo que se evalúan dichas mediciones ópticas;seleccionar, en base a dicha predicción, una combinación personalizada de los agentes activos para efectuar un tratamiento deseado de dicho cabello, estando al menos uno de dichos agentes activos formulado en forma de comprimido, y seleccionar dicha combinación que comprende seleccionar una combinación de dichos comprimidos;preparar una composición que comprende dicha combinación personalizada de agentes activos, en donde la preparación de dicha composición comprende distribuir dicha combinación de comprimidos a partir del dispositivo;y poner en contacto dicho cabello con dicha composición. 111
Independent claims12
1,801 paragraphs in 65 sections, as filed
ES 2 823 977 T3
DESCRIPTION
Systems for custom coloring
Field and background of the invention
The present invention, in some embodiments thereof, relates to methods and systems for treating keratinous fibers and, more particularly, though not exclusively, to tablet formulations for treating keratinous fibers, such as human hair, to a configured dispenser device. to supply tablet formulations, to an optical reader to obtain optical information from keratinous fibers, to a device and method to predict the results of a keratinous fiber treatment operation and to select an appropriate composition to treat keratinous fibers in accordance with the prediction and to systems for the personalized treatment of hair and other keratinous fibers using any of the formulations of tablet, dispenser device, optical reader and prediction device and method, either alone or in any combination.
Many people want to alter their appearance by using hair coloring. For this purpose, individuals either turn to professional salons or purchase ready-to-use preparations that can be self-applied by the user. In both cases, the customer identifies their desired color from a catalog, the appropriate colors or preparations are selected from a finite set of available shades, and the appropriate treatments are applied.
Hair colorants are made in many colors. Usually, a dye color is indicated on the box containing the colorant, either by a color number, a printed example of the color, or means of a colored hair curl sample.
However, the chemicals in the dye interact with the chemicals in uncoloured hair and optionally with the dye already present in the hair. Thus, even where the same colorant is used, the hair color after coloring differs considerably depending on the natural color or the natural color plus the mixture of the old hair dye before coloring. For example, in the case where the hair before coloring has an inhomogeneous mixture of white hair and colored hair, current methods fail to accurately predict the hair color after coloring. Also, in the case where naturally pigmented hair is already colored with artificial colors, the resulting color depends on the combination of original pigments and artificial pigments already present in the hair.
Consequently, it is difficult to predict the color that will result from coloring any of the person's hair solely from the impression of a box or a fixed sample of the hair, and a problem frequently arises in that the actual hair color after coloring is different from that of the hair. anticipated color.
Indeed, the matter is further complicated by the nature of the coloring process, which chemically changes the substances in the hair, including natural hair factors and artificial colors already present.
Various methods and systems have been developed to predict the final hair color in order to minimize errors and increase customer satisfaction with the use of hair color products. For example, US Patent No. 6,707,929 describes a method and system for analyzing hair and predicting available colored hair colors. This patent describes methods for identifying an obtainable hair color based on at least one receptor starting hair value, for identifying a hair coloring agent based on at least one receptor starting hair value, and emitting a image for a hair color analysis system. US Patent No. 6,707,929 further describes a method for providing a hair coloring product to a consumer, which is effected by identifying hair colors available to the consumer, illustrating the colors available to the consumer, allowing the consumer to select a desired hair color and recommend a hair coloring agent to the user to obtain the desired hair color.
Some systems to obtain the above are based on color coordinates. However, the color coordinates do not sufficiently take into account the natural materials in the hair. Improved systems that use a spectrum of the hair and make color calculations based on comparing the spectrum of the hair with the spectrum of the dye or dye mixture has therefore been developed.
However, even with spectral measurements there is not enough information to characterize hair and make effective predictions, since natural hair pigments tend to be highly absorbent of visible light and are thus difficult to distinguish.
Also, previous systems only manipulate the measured colors. As mentioned, hair coloring is a chemical process that involves highly active chemical components that have dynamic effects on the hair and on the substances. Thus the final results of the dyeing process depend not only on the colors used, but on the way in which these chemical processes are carried out. These processes can have a strong dependence on the values of the initial concentration of natural and artificial pigments, also
ES 2 823 977 T3 and the physical characteristics of the hair, such as its diameter, its permeability and the condition of the cuticles on its surface. These parameters impact both the rate at which chemical reactions take place and the amount of specular reflection that hair acquires after coloring, specular reflection providing the level of shine. There are different types of hair coloring on the market. A commonly used hair colorant is a permanent dye that achieves an essentially permanent dyeing effect through the oxidative coupling reaction of the dye within the hair (the cortex of the hair). A less permanent change in appearance can be obtained from temporary hair coloring of the hair hair surface and semi-permanent and demi-permanent coloring that provides intermediate dye penetrations and intermediate coloring durations.
Permanent hair coloring is usually obtained by oxidative hair coloring processes. Oxidizing hair coloring operates by penetration of a small molecule dye precursor (also known as a primary intermediate), and in many cases also a small molecule dye coupler (also known as a secondary intermediate), into the swollen hair by an agent. alkaline such as ammonia. After oxidation, either by addition of an oxidizing agent or for some dyes, by atmospheric oxygen, the dye precursors and couplers react with each other and / or by themselves to produce larger colored molecules which, due to their increased size , remain trapped inside the hair shaft. Direct dyes, such as azo dyes and HC nitro dyes, which themselves are commonly used for temporary coloring, are also used in some permanent hair coloring, often in addition to dye precursors and / or couplers.
In addition to facilitating oxidative coloring processes, oxidizing agents such as hydrogen peroxide can also bleach or lighten hair by destroying natural melamine pigments in the hair shaft.
In general, permanent hair colorants are commercially available in wet form. Such coloring preparations usually comprise a 'dye' element, comprising premixed color-imparting agents (dye precursors, dye couplers and / or direct dyes) in an alkaline medium and a 'developer' element comprising an oxidizing agent. Both elements are supplied in liquid to creamy or paste form and the two elements are combined immediately prior to application.
For home use and for salon use, the tint element is generally packaged in a single application container, such as a sealed tube, which reduces the exposure of the dyes to oxygen and light and / or the evaporation of pivotal agents such as like ammonia. The developer is less sensitive to degradation and can be supplied in separate tubes or bottles or in large multi-dose containers.
In addition to the stability issues inherent in the oxidative coloring process by currently used wet formulations of hair colorants, these one-shot dyes also suffer from limited flexibility or reproducibility and hence from limited options and limited accuracy. in cases where custom hair coloring is desired or required. Customers looking to use hair colorants want a host of color options, reflecting at least the wide range of natural hair colors.
The dye comprising the color-imparting agents may alternatively be supplied as a powder phoneme, which is mixed prior to use in an appropriate carrier comprising the necessary additional components. These dye forms exhibit improved stability compared to a liquid dye element, due to lower sensitivity to atmospheric oxygen. However, such powder coloring compositions must be protected from exposure to degradation factors to prevent premature deterioration.
US Patent No. 7,458,992 describes coated dye-containing beads.
International patent application PCT / US2009 / 046273 (published as WO 2009/152033) discloses a color query system for a beauty salon where hair colors in powder, granule or particle form are mixed according to the calculations of a processor in order to prepare a hair color treatment for a desired hair color.
US Patent No. 6,790,240 describes a formed body containing a dye precursor, an oxidizing agent and an alkaline agent, for preparing coloring compositions by placing the formed body in a composition containing water. Cellulose-based disintegrants such as microcrystalline cellulose are described for inclusion in the formed body.
US Patent No. 7,204,856 describes a shaped body containing a disintegration aid and a thickener to form preparations such as hair coloring preparations. Cellulose-based disintegration aids such as microcrystalline cellulose are described.
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US Patent Application having Publication No. 2005/0039271 describes a formed body, consisting of a dissolution accelerator and a second oxidation dye intermediate in a carrier for coloring keratinous fibers. The body formed is free of primary intermediate oxidation dye precursors. The dissolution accelerator can be a gas evoking component, a locked gas, a disintegration aid, or a mixture thereof. Cellulose-based disintegration aids such as microcrystalline cellulose are described.
US Patent Application having Publication No. 2003/0028978 describes a formed body containing at least one indole derivative and / or indoline derivative, for preparing coloring compositions by placing the formed body in a composition containing water. .
US Patent No. 5660342 describes a mixing device for mixing a liquid with a dry material, particularly a bleaching agent. The tablets of dry material are crushed and the broken pieces are then mixed with a liquid.
WO 2010/100231 describes a device for delivering a coloring composition for keratin fibers, wherein 20% of the coloring composition is an anhydrous oil-containing composition. The device comprises three reservoirs for supplying a dye composition, an oxidizing composition and the oil-containing composition, the compositions are supplied together in a package.
EP Patent No. 2081668 describes an apparatus for producing required quantities of cosmetic preparations. The basic preparations are transported with the help of electric pumps, from containers in the apparatus to a mixing chamber and the preparation is delivered immediately from the combination of the components thereof.
Additional prior art includes WO 2004/082650; WO 2004/058202; WO 2003/074015; WO 2001/45647; US Patent Application having Publication No. 2002/0194684; FR Patent No. 2901131; US Patent No. 5205837; EP Patent No. 0590538; WO 2009/121643; WO 2008/046518; and EP Patent No. 1817976.
Summary of the invention
According to one aspect of some embodiments of the present invention, there is provided an assembly according to claim 1.
In accordance with some embodiments of the present invention, the device further comprises a platform, the platform having the plurality of containers connected thereto.
According to some embodiments of the present invention, the containers and the dispenser unit are connectable to each other through the platform.
According to some embodiments of the present invention, the device further comprises at least one funnel configured to direct distributed tablets from the container to an outlet.
According to some embodiments of the present invention, the device further comprises one or more optional elements selected from the group comprising legs that support the platform, housings suitable for enclosing at least part of the device, pedestals for receiving containers suitable for containing the custom combination of tablets and user interfaces suitable for providing or retrieving information concerning the custom combination of tablets.
In accordance with some embodiments of the present invention, the device further comprises means for weighing or counting the tablets to thereby provide the predetermined quantity of the tablets to be dispensed from each of the containers.
In accordance with some embodiments of the present invention, each of the containers individually comprises a different type of tablets and wherein the personalized treatment composition comprises the predetermined amount of each of the at least one type of tablets.
In accordance with some embodiments of the present invention, the custom coloring composition comprises a combination of at least two different types of tablets, each of the types of tablets being supplied from a different container.
According to some embodiments of the present invention, at least one type of tablet comprises a coloration agent.
In accordance with some embodiments of the present invention, the device is configured to supply two or more
ES 2 823 977 T3 types of tablets, each comprising a different color-imparting agent, to thereby provide a predetermined range of color-imparting agents.
According to some embodiments of the present invention, at least one type of tablet comprises fast disintegration tablets.
According to some embodiments of the present invention, at least one type of tablet comprises an active agent selected from the group consisting of an oxidizing agent, an alkalizing agent, and a thickening agent.
In accordance with some embodiments of the present invention, the device is configured to generate at least one medium selected from the group consisting of an alkalizing medium, a bleaching medium, an oxidizing medium, and a thickening medium.
According to some embodiments of the present invention, the device further comprises at least one additional compartment that contains at least one of the media and is configured to supply each of the at least one media in a predetermined amount.
According to some embodiments of the present invention, the device further comprises at least one additional compartment comprising an aqueous solution and which is in communication with at least a part of the compartments and which comprises the at least one active agent, being the device configured to generate a predetermined amount of the medium upon contact of one type of the tablets with the aqueous solution.
According to some embodiments of the present invention, the device further comprises a mixing unit for mixing the tablets with the media.
According to some embodiments of the present invention, the device further comprises a printed circuit board for connecting the electronic components of the device.
The device further comprises at least one computer-implemented unit.
The computer-implemented unit (or means) interfaces with the dispensing unit of each of the containers and wherein the predetermined quantity of the tablets is selected by the computer-implemented unit.
The predetermined amount of the tablets is selected by the computer implemented means (unit) taking into account the initial properties of the hair.
Taking into account the initial properties, this is done by means of an optical measuring instrument.
According to some embodiments of the present invention, the optical measuring instrument comprises:
a lighting unit to illuminate the hair;
a measurement unit comprising at least one sensor for optically measuring hair during illumination by the illumination unit; wherein the sensor and a beam from the lighting unit use, respectively, wavelengths in the visible and infrared spectral regions, thereby providing a hair spectrum that distinguishes both between different natural hair colorants and between different artificial hair coloring.
According to some embodiments of the present invention, tablets and suitable media are supplied in the form of a multi-component kit.
According to some embodiments of the present invention, at least one type of the tablets comprises a solid formulation, as described herein.
In accordance with some embodiments of the present invention, each of the tablets is a solid formulation, as described herein.
In accordance with one aspect of some embodiments of the present invention, there is provided a method for performing a personalized hair treatment in accordance with claim 12.
Preparation of the composition comprises dispensing the combination of tablets from a dispensing device.
The distributor device interfaces with the computer implemented unit.
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In any of the above aspects, active agents include color-imparting agents, thickening agents, oxidizing agents, and / or alkaline agents.
In any of the above aspects, the selection is in addition to conditions for contacting the composition with the hair, where the conditions include, but are not limited to, speed, duration and temperature.
In accordance with one aspect of some embodiments of the present invention, a solid formulation suitable for use in treating hair is provided, the formulation is in tablet form and comprising at least one water-soluble super-disintegrating agent and at least one agent. active selected from the group consisting of a color-imparting agent, an alkaline agent, an oxidizing agent, and a thickening agent, the super-disintegrating agent is characterized by a water absorption ratio of at least 0.5.
In accordance with some embodiments of the present invention, the solid formulation is for use in preparing a composition for treating hair.
According to some embodiments of the present invention, the hair treatment composition is a coloring composition.
According to some embodiments of the present invention, the super-disintegrating agent is characterized by a water absorption ratio ranging from 0.5 to 2.
According to some embodiments of the present invention, the superdisintegrating agent is characterized by a water absorption ratio ranging from 0.6 to 0.9.
According to some embodiments of the present invention, the super-disintegrating agent is a cross-linked polymer.
In accordance with some embodiments of the present invention, the superdisintegrating agent is selected from the group consisting of croscarmellose, crospovidone, cross-linked starch, cross-linked alginic acid, cross-linked polyacrylic acid, and a polysaccharide.
In accordance with some embodiments of the present invention, the superdisintegrating agent is selected from the group consisting of croscarmellose, crospovidone, and cross-linked starch.
In accordance with some embodiments of the present invention, the at least one water-insoluble superdisintegrating agent is in a concentration in a range of 0.1 to 10 percent by weight of the tablet when uncoated.
In accordance with some embodiments of the present invention, the at least one water-insoluble superdisintegrant is in a concentration in a range of 0.5 to 5 percent by weight of the tablet when uncoated.
According to some embodiments of the present invention, the at least one active agent comprises at least one color-imparting agent.
According to some embodiments of the present invention, the at least one active agent comprises at least one color-imparting agent.
In accordance with some embodiments of the present invention, the color-imparting agent is selected from the group consisting of a dye precursor, a dye coupler, a direct dye, and any combination thereof.
In accordance with some embodiments of the present invention, the at least one active agent is selected from the group consisting of a direct dye and a combination of at least one dye precursor and at least one dye coupler.
According to some embodiments of the present invention, the molar ratio of at least one dye precursor and at least one dye coupler ranges from 2: 1 to 1: 2 and is preferably less than 1.
According to some embodiments of the present invention, the at least one active agent comprises at least one alkaline agent.
According to some embodiments of the present invention, the at least one active agent comprises at least the alkaline agent.
According to some embodiments of the present invention, the at least one active agent comprises at least one oxidizing agent suitable for bleaching hair.
According to some embodiments of the present invention, the at least one active agent comprises at least one
ES 2 823 977 T3 oxidizing agent.
According to some embodiments of the present invention, the at least one oxidizing agent is suitable to react with a dye precursor to form a dye.
According to some embodiments of the present invention, the active agent comprises at least one thickening agent.
According to some embodiments of the present invention, the solid formulation further comprises ascorbic acid.
According to some embodiments of the present invention, the solid formulation further comprises at least one excipient.
In accordance with some embodiments of the present invention, the solid formulation has a water content of less than 3 percent by weight.
According to some embodiments of the present invention, the tablet further comprises a coating.
According to some embodiments of the present invention, the coating comprises at least one coloring agent.
According to some embodiments of the present invention, the coating has a thickness in a range of 5 µm to 50 µm.
According to some embodiments of the present invention, the tablet has a maximum width in a range of 2mm to 10mm.
According to some embodiments of the present invention, the solid formulation is substantially spherical or spheroidal and has an average diameter in a range of 3mm to 7mm.
According to one aspect of some embodiments of the present invention, a composition suitable for use in treating hair is provided, the composition comprising an aqueous medium and at least one solid formulation as described herein disaggregated in the medium.
In accordance with some embodiments of the present invention, the composition is characterized by an appropriate viscosity to provide sufficient contact time between the composition and the fibers.
According to some embodiments of the present invention, the composition is suitable for coloring human hair.
In accordance with some embodiments of the present invention, the composition comprises a plurality of disintegrated tablets, the plurality of tablets customizing the hair coloring of an individual subject.
In accordance with one aspect of some embodiments of the present invention a hair treatment kit is provided, the kit comprising at least one set of a plurality of solid formulations as described herein, the at least one set consisting of a plurality of substantially identical solid formulations.
According to some embodiments of the present invention, the kit comprises at least three of the sets of solid formulations, each of the sets comprises a color-imparting agent, wherein the color-imparting agents are different from each other in each of the sets.
According to some embodiments of the present invention, the kit further comprises at least one aqueous medium enclosed in a container, the medium is selected from the group consisting of an oxidizing medium, an alkalizing medium, and a carrier medium.
According to some embodiments of the present invention, the at least one aqueous medium is suitable for disintegration of tablets.
According to some embodiments of the present invention, the kit further comprises at least one additional set of solid formulations, wherein the active agent in the solid formulations in the additional set comprises an alkaline agent.
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In accordance with some embodiments of the present invention, sets of solid formulations are customized for the coloring of the hair of an individual subject.
In accordance with one aspect of some embodiments of the present invention, there is provided a method for preparing the solid formulation as described herein, the method comprising:
forming a mixture comprising the at least one active agent and the at least one superdisintegrant and compressing the mixture, to thereby form the tablet.
According to some embodiments of the present invention, the mixture comprises a plurality of particles and wherein at least 80% by weight of the particles have a diameter of 200 µm or less.
In accordance with some embodiments of the present invention, the method further comprises coating the tablet.
In accordance with some embodiments of the present invention, the method further comprises drying the tablet.
In accordance with one aspect of some embodiments of the present invention, a method of treating hair is provided, the method comprising:
disintegrating at least one solid formulation as described herein in a first aqueous medium, to thereby obtain a composition comprising the at least one active agent and contacting the composition with the hair for an appropriate period of time to treat The hair.
According to some embodiments of the present invention, the at least one solid formulation comprises at least one color-imparting agent, the method of being coloring the hair.
In accordance with some embodiments of the present invention, the method further comprises, prior to contact of the composition with the fibers, contacting the fibers with a bleaching medium for a period of time sufficient to lighten the color of the fibers.
In accordance with some embodiments of the present invention, the method further comprises preparing the bleaching medium by disintegrating at least one solid formulation comprising an oxidizing agent in an aqueous medium.
According to some embodiments of the present invention, the method further comprises mixing the at least one solid formulation before, during and / or after disintegration with an active agent selected from the group consisting of an alkaline agent, an oxidizing agent and a thickener.
According to some embodiments of the present invention, the method comprises mixing the at least one solid formulation with an oxidizing medium, the oxidizing medium comprising at least one oxidizing agent and an appropriate carrier, wherein the concentration of the at least one oxidizing agent in the oxidizing medium it is in a range from 0.5 to 25% by weight.
According to some embodiments of the present invention, the method comprises mixing the at least one solid formulation with an alkalizing medium, the alkalizing medium comprises at least one alkaline agent and an appropriate carrier, wherein the concentration of the at least one alkaline agent in the alkalizing medium is in a range of 0.1 to 15% by weight.
According to some embodiments of the present invention, the method further comprises selecting the at least one solid formulation from a plurality of solid formulations of different types, wherein the selection comprises:
establish the initial properties of the hair;
selecting a desired personalized treatment appropriate for an individual subject and determining the amount of the solid formulations of each of the appropriate types in combination, to effect the desired personalized treatment.
According to some embodiments of the present invention, the custom treatment comprises custom coloring and wherein establishing the initial properties comprises measuring an initial reflectance spectrum and selecting the custom color comprises determining the reflectance spectrum of the custom color, wherein the Reflectance spectra are independently converted to a color coordinate display.
According to some embodiments of the present invention, determining the amount of solid formulations comprises:
add to the display of color coordinates of the initial reflectance spectrum the positive contribution or
ES 2 823 977 T3 negative of a solid formulation comprising a color-imparting agent that provides a basic shade to the presentation of color coordinates, thereby calculating an intermediate color coordinate display and iterating the calculation of the intermediate color display after adding a solid formulation comprising the color-imparting agent and after replacing the solid formulation with a formulation comprising a color-imparting agent different, until the difference between the intermediate color coordinate display and the desired color coordinate display is minimized.
According to some embodiments of the present invention, the determination further takes into account the positive and / or negative contribution of at least one active agent selected from the group consisting of an alkaline agent, an oxidizing agent, and a thickening agent on the hair to the computed color coordinate display.
According to some embodiments of the present invention, the selection further takes into account the contribution of individual properties of the hair.
In accordance with some embodiments of the present invention, the selection is performed by one or more computer-implemented systems.
According to some embodiments of the present invention, the selection uses a prediction, the prediction of a result of a hair treatment using a predetermined composition, the prediction comprising:
measure an initial spectrum of the hair;
determining from the initial spectrum the presence and concentration of respective fiber constituents;
determining the modified concentration of the fiber constituents following the bleaching effects of chemical agents in the composition;
determine the final concentrations of the fiber constituents following the interaction of the chemical agents with dyes in the fiber and from the final concentrations, predict the final fiber spectrum from which the treatment result can be calculated.
According to some embodiments of the present invention, determining the initial spectrum of the presence and concentration of respective fiber constituents comprises calculating, from the initial spectrum, the presence and initial concentration of keratin, eumelanin, pheomelanin, and artificial pigments and / or where the determination of the modified concentration comprises:
from the predetermined recipe obtaining factors for the alkaline agent concentration, hydrogen peroxide concentration, temperature, hair diameter, condition of the hair and its cuticles, ethnicity and duration of exposure;
from at least some factors obtained, determine the modified concentrations of keratin, eumelanin and pheomelanin or from the predetermined recipe obtain a dye concentration factor and from at least some of the factors for the dye concentration and at least some of the alkaline agent concentration, hydrogen peroxide concentration, temperature, hair diameter, condition of the hair and its cuticles, ethnicity and duration of exposure, determine the final concentration of the artificial dye or where the prediction of the final spectrum of the hair comprises, make the prediction from the final concentrations of the artificial dye, keratin, eumelanin and pheomelanin, predicting a final spectrum of the hair or where the relationship between ingredient concentrations and final spectra is determined in the Kubelka Munk formula.
According to some embodiments of the present invention, the Kubelka Munk approximation is of the form:
(1 -^))<sup>2</sup><sub>=</sub>
2 - /? W where:
R (A) = The diffuse reflectance at the wavelength;
Κ (λ)<sub>η</sub> = The absorption in wavelength, of n <sup>th</sup> ingredient;
ES 2 823 977 T3
S (A)<sub>n</sub> = The dispersion, in wavelength, of n <sup>th</sup> ingredient and
C<sub>n</sub> = The concentration of n <sup>th</sup> Colorant.
According to some embodiments of the present invention, the wavelength diffuse reflectance -R (A) -is obtained from the Sanderson correction formula.
According to some embodiments of the present invention, predicting a final spectrum or determining the respective hair constituents comprises correcting for specular reflection effects and correcting for specular reflection effects comprises considering an air-to-hair boundary and a frontier of external reaction of hair to internal reaction of hair and / or the correction comprises applying a Sanderson correction.
According to some embodiments of the present invention, the Sanderson correction is of the form:
where:
A = wavelength a = The relative portion of specular reflectance that propagates to the spectrometer detector;
R (A) = Reflectance corrected by Saunderson's formula;
F (A) ext = The external (specular) Fresnel reflectance of the external side of the hair;
F (A) ¡nt = The internal Fresnel reflectance between the internal of the hair and the border region of the hair.
According to some embodiments of the present invention, the reflectance corrected according to the Sanderson correction -R (A) - is inserted to the Kubelka Munky / or approximation where the modified or final concentrations of keratin, in melanin, eumelanin , pheomelanin and artificial dye are calculated using a chemical reaction kinetic equation, where the calculation of the final concentrations also considers taking into account intermediate products that appear from chemical reactions.
According to some embodiments of the present invention, the measurement is performed by an optical hair measuring device for measuring optical hair comprising:
a lighting unit to illuminate the hair;
a measuring unit comprising at least one sensor for optically measuring hair during illumination by the illumination unit; wherein the sensor and the lighting unit beam are respectively obtained where a light diffusion angle in the medium is measured, thereby ensuring that the driver mainly measures the light from the illumination beam that is diffuse or scattered by The hair.
In accordance with some embodiments of the present invention, the device further comprises a main light source and subsidiary light sources and processing electronics for using differential lighting results from respective sources to determine an angle of the hair relative to the light source. main lighting.
In accordance with some embodiments of the present invention, at least the main illumination source is used for spectroscopy and at least one subsidiary illumination source is used for angle measurement.
According to some embodiments of the present invention, the sensor comprises sensitivity to the visible near infrared portions of the electromagnetic spectrum.
In accordance with one aspect of some embodiments of the present invention, a method is provided for predicting the outcome of a keratinous fiber treatment using a predetermined composition comprising:
measure the initial spectrum of keratinous fibers;
determining from the initial spectrum the presence and concentration of the respective fiber constituents;
determining the modified concentrations of the fiber constituents following the bleaching effects of the chemical agents in the composition;
determine the final concentrations of fiber constituents following the interaction of chemical agents with dyes in the fiber and
ES 2 823 977 T3 from the final concentrations, predict spectrum of the fiber from which the treatment result can be calculated.
According to some embodiments of the present invention, determining from the initial spectrum the presence and concentration of respective fiber constituents comprises calculating from the initial spectrum the presence and initial concentrations of keratin, eumelanin, pheomelanin, and artificial pigments.
According to some embodiments of the present invention, the determination of the modified concentration comprises:
from the predetermined recipe obtain factors for the concentration of the alkaline agent, oxidant concentration, temperature, diameter of the hair, condition of the hair and its cuticles, ethnicity and duration of exposure;
From at least some of the factors obtained, determine the modified concentrations of keratin, eumelanin and pheomelanin or from the predetermined recipe obtain a dye concentration factor and from at least some of the factors for the dye concentration and at minus some of the alkaline agent concentration, oxidizing agent concentration, temperature, hair diameter, condition of the hair and its cuticles, ethnicity and duration of exposure, determining the final concentration of the artificial dye or where the prediction of the final spectrum of the keratinous fibers comprises making the prediction from the final concentrations of the artificial dye, keratin, eumelanin and pheomelanin, predicting a final spectrum of the keratinous fibers or where the relationship between ingredient concentrations and final spectra is determined in the Kubelka Munk formula.
According to some embodiments of the present invention, the Kubelka Munk approximation is of the form:
(1 - RW)<sup>2</sup> Σ ”= 1 c„ Α '(Λ) „« (1) C „S (2)„ as defined herein.
According to some embodiments of the present invention, the wavelength diffuse reflectance -R (A) -is obtained from the Sanderson correction formula.
According to some embodiments of the present invention, predicting the final spectrum or determining the respective hair constituents comprises correcting for specular reflection effects.
In accordance with some embodiments of the present invention, correction for specular reflection effects comprises considering an air-to-keratinous fiber boundary and a keratinous fiber outer region to keratinous fiber inner region fiber.
According to some embodiments of the present invention, the correction comprises applying a Sanderson correction.
According to some embodiments of the present invention, the Sanderson correction is of the form:
- a χ η χ χ .Λ iZitrUj as defined herein.
According to some embodiments of the present invention, the reflectance corrected according to the Sanderson correction -R (A) - is inserted to the Kubelka Munk approximation.
According to some embodiments of the present invention, the modified or final concentrations of keratin, eumelanin, pheomelanin and artificial dye are calculated using a chemical reaction kinetics equation, where the calculation of the final concentrations also considers taking into account intermediates. that appear from chemical reactions.
In accordance with one aspect of some embodiments of the present invention, a method is provided for predicting
ES 2 823 977 T3 resulting from a keratinous fiber treatment using a predetermined composition, the method comprising:
measure the initial spectrum of keratinous fibers;
from the initial concentrations of natural factors of the fibers and of factors obtained from the predetermined composition to predict a final spectrum of the fibers after the treatment;
correcting the final spectrum for specular reflection effects;
further correct the final spectrum corrected for specular correction effects with an additional correction for light effects.
According to some embodiments of the present invention, correction for specular reflection effects comprises considering an air-to-keratinous fiber boundary and an outer keratinous fiber-to-inner region keratinous fiber reaction boundary, wherein the correction comprises applying a correction of Sanderson and where the Sanderson correction formula comprises:
as defined herein.
According to some embodiments of the present invention, the reflectance corrected according to the Sanderson correction -R (A) - is inserted to the Kubelka Munk approximation.
According to some embodiments of the present invention, the final spectrum is obtained by calculating the final concentrations of keratin, eumelanin, pheomelanin and artificial dye from the initial concentrations using a chemical reaction kinetic equation and where the calculation of The final concentrations also consider taking into account intermediate products that appear from chemical reactions.
According to one aspect of some embodiments of the present invention, the method further comprises providing a tablet to obtain the final spectrum, the tablet comprising at least one water-insoluble super-disintegrating agent that swells on contact with water and at least one agent active selected from the group consisting of a color imparting agent, an alkaline agent, an oxidizing agent, and a thickening agent.
According to some embodiments of the present invention, the method further comprises obtaining optical measurements of keratinous fibers, comprising obtaining:
apply a light source to the keratinous fibers;
optically measure the illumination of the keratinous fibers of a diffusion angle in relation to the illumination source, the illumination angle falls between 45 degrees and 135 degrees, to obtain by this a measurement whose main components are light that has been scattered or scattered by the hair of the light source.
In accordance with one aspect of some embodiments of the present invention, a system is provided for predicting the outcome of a keratinous fiber treatment and preparing a composition therefor, the system comprising:
a spectrometer to measure the initial spectrum of keratinous fibers;
a constituent estimation unit for determining from the initial spectrum the presence and concentration of constituents of the respective hair;
a kinetic chemical reaction modeling unit to a) determine the modified concentration of keratinous fiber constituents following the bleaching effects of chemicals in the recipe and b) determine the final concentrations of keratinous fiber constituents following the interaction of chemical agents with dyes and keratinous fibers and a spectral prediction unit to use the final concentrations to predict the final spectrum of the fiber and a mixing unit to prepare the appropriate composition for treatment if the final spectrum is approved.
According to one aspect of some embodiments of the present invention, the keratinous fibers are the subject's hair and the subject's hair is initially hair that has natural coloration near the roots or hair that has natural coloration away from the roots or the subject's hair is initially hair that has artificial coloration or initially hair that have white coloring or initially hair that contains residue from treatment with chemical perming or waving compounds.
In accordance with one aspect of some embodiments of the present invention, a device is provided for
ES 2 823 977 T3 optical measurement of keratinous fibers comprising:
a lighting unit for illuminating keratinous fibers;
a measurement unit comprising at least one sensor to optically measure the keratinous fibers during illumination by the illumination unit; wherein the sensor and one of the illumination unit respectively obtain a light diffusion angle in the keratinous fibers which are measures to ensure by this that the sensor mainly measures light from the illumination beam that is diffused or scattered by the keratinous fibers.
According to some embodiments of the present invention, the measurement unit comprises a plurality of sensors located around the keratinous fibers at an elevation of the azimuth and the illumination unit is positioned perpendicular to the keratinous fibers.
In accordance with some embodiments of the present invention, the illumination unit comprises a plurality of illumination sources respectively configured to illuminate the keratinous fibers from a plurality of substantially azimuthal angles.
According to some embodiments of the present invention, the angle of light scattering is between 45 and 135 degrees.
In accordance with some embodiments of the present invention, the illumination unit comprises two substantially opposite illumination directions along the hair axis, such that a differential comparison between detections of each respective direction provides an indication of a condition of a hair scapula.
According to some embodiments of the present invention, the illumination unit comprises a light source parallel to the axis of the keratinous fibers or at least two illumination sources, wherein at least two of the illumination sources illuminate the keratinous fibers from angles respectively different azimuths.
In accordance with some embodiments of the present invention, the illumination sources are configured to illuminate the keratinous fibers at different times, thereby allowing the illumination of respective sources to be measured separately.
According to some embodiments of the present invention, the device further comprises a main light source and subsidiary light sources and processing electronics to use differential tilt results from respective sources to determine the angle of the hair relative to the main light source or the processing electronics are configured to use the angle of the keratinous fibers to correct the spectrum of the keratinous fibers or components Processing electronics are configured to use differential illumination results from multiple illumination sources to distinguish between specular and diffuse light from keratinous fibers or where at least the primary illumination source is used for spectroscopy and at least one illumination source. Subsidiary is used for angle measurement or where at least a second illumination source is used for spectroscopy.
According to some embodiments of the present invention, there are four illumination sources at the same elevation angle relative to a plane perpendicular to a detection axis and where an azimuth angle relative to an axis of keratinous fibers is 30 ° for two of the four light sources and 150 ° for a third and a fourth of the light sources.
According to some embodiments of the present invention, the sensor comprises sensitivity to the visible and near infrared portions of the electromagnetic spectrum or wherein the sensor comprises sensitivity to at least the wavelength range of 350-1,500 nm or wherein the sensor comprises sensitivity to wavelength ranges of 350-750 nm or wherein the sensor comprises sensitivity to at least a wavelength range of 400-950 nm or wherein the sensor comprises at least one calibration region for receiving light from calibrating and calibrating the optical readings or the device further comprises a controllably polarizing element or further comprises a controllably analyzing element or further comprises fasteners to hold keratinous fibers and imposition for measurement.
In accordance with some embodiments of the present invention, there is provided a keratinous fiber optical measurement device comprising:
a lighting unit for illuminating keratinous fibers;
a measurement unit comprising at least one sensor for optically measuring keratinous fibers during illumination by the illumination unit; wherein the sensor and a beam from the illumination unit respectively use wavelengths in the visible and infrared spectral regions, to thereby provide a spectrum of keratinous fibers that discriminates both between different natural dyes and the fibers
ES 2 823 977 T3 keratinous fibers and among different artificial colorants in keratinous fibers.
According to some embodiments of the present invention, the sensor comprises sensitivity to at least the wavelength range of 350-1,500 nm or wherein the sensor comprises sensitivity to wavelength ranges of 350-750 nm or wherein the sensor comprises sensitivity to at least the wavelength range of 400-950nm waveform or wherein the sensor comprises at least one calibration region to receive calibration light and calibrate optical readings or comprises at least one known calibrated target to allow calibration real-time internal calibration for each measurement or comprises two known calibrated targets to enable real-time internal calibration for different light illumination power.
In accordance with one aspect of some embodiments of the present invention, a method is provided for obtaining optical measurements of keratinous fibers comprising:
apply a light source to the keratinous fibers;
optically measure the illumination of keratinous fibers from a diffusion angle in relation to the illumination source, the illumination angle falls between 45 degrees and 135 degrees, to obtain by this a measurement whose main components are light that has been scattered or scattered by the keratinous fibers of the light source.
According to some embodiments of the present invention, the method comprises illuminating the keratinous fibers of a plurality of illumination sources at a plurality of angles in sequence including respectively opposite angles and obtaining differential measurements of the opposite angles.
Unless defined otherwise, all technical and / or scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art with which the invention is concerned. Although similar methods and materials equivalent to those described herein may be used in the practice or testing of embodiments of the invention, exemplary methods and / or materials are described below. In case of conflict, the patent specification, including definitions, will prevail. Furthermore, the materials, methods, and examples are illustrative only and are not intended to be necessarily limiting.
Implementation of the method and / or device in accordance with some aspects of embodiments of the invention may involve performing or consuming selected tasks manually, automatically, or a combination of both. Furthermore, according to the actual instrumentation and equipment of embodiments of the method and / or device of the invention, several selected tasks could be implemented by physical elements, by programming elements or by fixed elements or by a combination thereof using a system. operational.
For example, to perform selected tasks according to embodiments of the invention they could be implemented as a chip or a circuit. As programming elements, the selected tasks in accordance with embodiments of the invention could be implemented as a plurality of programming element instructions that are executed by a computer using any appropriate operating system. In some embodiments of the invention, one or more tasks according to some embodiments of a method and / or device as described herein are performed by a data processor such as a computing platform to execute plurality of instructions. Optionally, the data processor includes volatile memory for storing instructions and / or data and / or non-volatile storage, for example a magnetic hard disk and / or removable media for storing instructions and / or data. Optionally, a network connection is provided as well. A display and / or a user input device such as a keyboard or mouse are optionally provided as well.
Brief description of the figures
Some embodiments of the invention are described herein by way of example only with reference to the accompanying figures. With specific reference now to the figures in detail, it is emphasized that the features shown are by way of example only and for purposes of illustrative discussion of embodiments of the invention. In this regard, the description taken with the figures becomes apparent to those skilled in the art as to how embodiments of the invention can be practiced.
In the figures:
Figure 1 is a detailed view of a dispenser device in accordance with exemplary embodiments of the invention;
Figure 2 shows a detailed view and a perspective view of a dispenser device in accordance with alternative exemplary embodiments of the invention;
Figures 3A-E show various possible container combinations on the platform of the dispenser device according to some exemplary embodiments of the invention;
Figure 4A-D show various possible types of containers according to some exemplary embodiments of the invention;
Figure 5 shows a detailed view and a cross-sectional view of a container and a dispenser element in accordance with exemplary embodiments of the invention;
Figure 6 shows a detailed view and a cross-sectional view of a container and dispenser element in accordance with alternative exemplary embodiments of the invention;
Each of Figures 7A-B shows a top view of a multi-compartment container with various combinations of internal containers in accordance with exemplary embodiments of the invention;
Figure 8 shows a top view of a dispenser element in accordance with exemplary embodiments of the invention;
Figures 9A-B present images of an exemplary coated tablet formulation according to some embodiments of the present invention (tablet # 15 in IE example) in 6% (w / w) hydrogen peroxide solution at t = 0 (figure 9A) and t = 3 seconds (figure 9B);
Figures 10A-B are images of exemplary coated tablets comprising a polyvinyl alcohol coating with pigment green 7 (Figure 10A) or pigment yellow 73 (Figure 10B);
Figure 11 is a light microscopy image of a coated tablet in which the coating thickness (length) is measured in two regions in order to obtain an average value;
Figure 12 is a graph showing the average coating thickness as measured in 10 measurements for 5 tablets tested each time, the average thickness of the tablets being 13.12 microns, with the error bars showing the deviation of the coating thickness for each measurement and the dotted line shows the envelope of two standard deviations around the average value of the coating thickness, in which the thickness of 95% of the tablets is covered;
Figures 13A-F present images showing the lightfastness of exemplary coated tablets according to some embodiments of the present invention at t = 0 (Figure 13A) and after one month (Figure 13B), after 3 months ( Figure 13C), after 6 months (Figure 13D), after 9 months (Figure 13E) and after one year (Figure 13F) of illumination.
Figure 14 is a graph showing the chromatographic separation of exemplary agents by HPLC;
Figures 15A-I show images of colored fibers with tablets and methods according to various embodiments of the invention;
Figures 16A-B show natural dark blonde Caucasian hair colored with an exemplary green hue formulation at different concentrations (Figure 16A) and yak hair colored by combinations of an exemplary orange hue formulation and an exemplary violet hue formulation (Figure 16A). 16B) at orange: violet ratios of 1: 100 (sample 1), 100: 1 (sample 2), and 100: 100 (sample 3).
Figure 17 is an image of human natural red hair without coloration (upper segment of the hair sample) with red-copper coloration (middle segment) and with coloration using an exemplary violet hue formulation in addition to the red-copper coloration;
Figure 18 is a simplified flow chart illustrating the operation of a hair color prediction methodology in accordance with one embodiment of the present invention;
Figure 19 is a simplified graph showing eumelanin kinetics during hair dyeing for different ammonia concentrations in a fixed duration, fixed hydrogen peroxide environment;
Figure 20 is a simplified graph showing the kinetics of eumelanin concentration during hair dyeing for different hydrogen peroxide concentrations in a fixed ammonia environment and duration;
Figure 21 is a simplified graph showing the kinetics of eumelanin concentration during hair dyeing for different durations in a fixed ammonia and hydrogen peroxide environment;
ES 2 823 977 T3 Figure 22 is a simplified graph showing the raven of the best fit to the measurement of natural hair spectra by optimizing the eumelanin concentration and pheomelanin concentration using the Kubelka Munk formula and Saunderson coefficients;
Figure 23 is a simplified graph of the best fit curve calculated by Kubelka Munk and the Saunderson correction for natural hair coloring with a known dye recipe that seeks to fit the curve of another measurement;
Figure 24 is a simplified graph illustrating the spectral square difference distribution after optimization in accordance with one embodiment of the present invention;
Figure 25 is a simplified graph illustrating the color coordinate distribution (dE) after optimization of natural undyed hair coloring in accordance with one embodiment of the present invention Figure 26 is a simplified graph illustrating the distribution square spectral differences after optimization of coloring of dyed hair in accordance with one embodiment of the present invention;
Figure 27 illustrates staining against hope for a series of samples;
Figure 28 is a simplified graph showing the kinetics of eumelanin concentration versus ammonia concentration, for fixed hydrogen peroxide and duration;
Figure 29 is a simplified graph showing the kinetics of eumelanin concentration versus hydrogen peroxide rate in the case of a model for initially colored hair, by fixed duration and fixed ammonia diffusion rate;
Figure 30 is a simplified graph showing the kinetics of eumelanin concentration versus duration while the ammonia rate and hydrogen peroxide rate were held constant and Figure 31 is a simplified flow chart showing a process to extract natural hair ingredient factors for calculation.
Figure 32A is a simplified schematic diagram showing an embodiment of the present invention in which hair is illuminated from azimuth and light is detected from perpendicular;
Figure 32B is a simplified schematic diagram showing a variation of the embodiment of Figure 32A in which hair is illuminated from perpendicular and light is detected from azimuth;
Figure 32C is a diagram showing optical elements for the illumination and measurement units of Figures 32A and 32B.
Figure 33A is a simplified schematic block diagram illustrating in greater detail the illumination and light gathering angles relative to the hair being measured for the embodiment of Figure 32A;
Fig. 33B is a schematic diagram showing illumination of a hair from two opposite directions of oblique lifting and light gathering to a perpendicular of the hair on the illumination side in accordance with the embodiment of Fig. 32A;
Fig. 33C is a schematic diagram showing hair illumination according to Fig. 33B viewed from above;
Figure 34A is a simplified side view of a hair reader in accordance with one embodiment of the present invention.
Figure 34B is a top view of the hair reader of Figure 34A;
Figure 35A shows hair with a noticeable cuticle where high scattering intensity is expected for the right side illumination and low scattering intensity for the left side;
Figure 35B shows hair in which the cuticle is smooth and the spread on the two sides would commonly be the same;
Figure 36 is a simplified graph showing two typical hair spectra as percentages of reflection in the range 350-1550 nm;
Figure 37 is a simplified graph illustrating the measured reflectance powers of blonde hair at different measurement angles;
Figure 38 is a simplified schematic diagram illustrating mechanical design elements of an embodiment of a hair reader in accordance with the present invention;
Figure 39A is a simplified diagram illustrating calibration using two calibration areas on the sensor in accordance with one embodiment of the present invention;
Figure 39B illustrates a block diagram showing hair illumination in a given polarization and passing the same polarization in the detection module, in accordance with one embodiment of the present invention and Figure 39C is a block diagram showing illumination of the hair in a given polarization and passing from orthogonal polarization in the detection module in accordance with one embodiment of the present invention;
Figure 40 is a detailed view of a dispenser device in accordance with embodiments of the present invention;
Fig. 41 is a side view showing a container according to an embodiment of the present invention with a perforated rubber cap attached to and detached from the dispenser;
Figure 42 is a side view and detailed diagram of a dispenser mechanism in accordance with embodiments of the present invention;
Figure 43 is a simplified diagram illustrating a container with partial spherical covers in accordance with one embodiment of the present invention;
Fig. 44 is a simplified diagram showing a cross section of the tablet dispenser according to one embodiment of the present invention;
Figure 45 is a simplified diagram showing replacement containers and mechanism in accordance with one embodiment of the present invention;
Figure 46 is a simplified diagram showing a media distribution mechanism in accordance with one embodiment of the present invention and Figure 47 is a simplified block diagram illustrating the different elements of the present embodiments working together.
Description of specific embodiments of the invention
The present invention deals with hair coloring. Various embodiments are concerned with methods and systems for treating hair and more particularly though not exclusively with tablet formulations for treating hair such as human hair, with an optical reader to obtain optical information from the hair, with a device and method for predicting the results of a hair treatment operation and for selecting a composition for treating hair in accordance with the prediction and with systems for personalized coloring of hair and other hair using any of the tablet formulations , optical reader and prediction device and method, either alone or in any combination.
Before explaining at least one embodiment of the invention in detail, it will be understood that the invention is not necessarily limited in its application to the details summarized in the following description or exemplified by the examples. The invention is capable of other embodiments or of being practiced or carried out in various ways.
The present inventors have successfully devised and prepared and implemented novel systems and methods for effecting the treatment (eg, coloring) of hair. These methods and systems comprise a dispensing device that is configured to provide a ready-to-use composition to treat hair (e.g., a coloring composition) and optionally, which is configured to provide a predetermined ready-to-use composition designed to suit the hair. default treatment (for example, default coloring effect; custom treatment).
The dispenser device can optionally be in communication with one or both of an optical reader, which determines the chemical and physical characteristics of the hair to be treated and computational means (means or computer-implemented unit) to determine the components and their concentrations. required to provide the predetermined composition and optionally or alternatively, to determine the proportion, duration and
ES 2 823 977 T3 temperature to apply the various active agents in the composition. When used in combination, the optical reader and the computational means are designed in such a way that the determination of the components and their concentrations in the compositions is made while considering the chemical and physical characteristics of the keratinous fibers to be treated and the desired result to be obtained, from here to provide a personalized treatment.
Accordingly, embodiments of the present invention are concerned with an optical reader to obtain sufficient characteristics of the hair to allow a real prediction of the result of a treatment (eg, color treatment) to be made. An optical reader can be a portable tool that measures the optical characteristics of the hair, which can then be used to calculate various characteristics of the fibers based on these parameters. The parameters can be used to support planning and recommendation of a treatment procedure or to support estimation of the outcome of the treatment procedure.
Some of the present embodiments are concerned with providing an optical reader that uses scattered and diffuse light and specular reflection of the hair being measured, since this gives more accurate measurements that are more useful for prediction and allows information to be obtained about the condition of the fibers which also contributes to the final appearance. Furthermore, the present embodiments can obtain spectral readings beyond visible ranges, where different natural pigments of the fibers are more easily distinguished. The result provides a significant improvement in the ability to accurately predict the effect of a given treatment on the hair.
The optical reader can use diffuse and / or scattered light and take measurements at multiple angles and / or multiple polarizations. Measurements at different angles and / or polarizations can then be compared. Illumination with different illumination characteristics at different times and / or at different positions through the measured hair allows readings at different angles and / or different wavelengths and / or different polarizations to be distinguished.
The optical reader is designed to distinguish in its operation between diffuse light from the internal part of the stem of the fibers that gives information regarding the color of the fibers and internal ingredients and scattering of light from the external surface of the stem that gives information concerning with the condition of the fibers.
Relative amounts of water in hair or treatment kinetic effects can be detected as will be explained.
The spectral range of the optical reader is beyond the visible and readings in the IR spectrum are used to help compensate for the strong absorption of melanin at visible wavelengths.
Both eumelanin and pheomelanin absorb much less light in IR than in visible. Two different stalks of fibers that are saturated with melanin but actually have different concentrations of melanin give very low reflectance intensity in the visible which is not much more than system noise making it difficult to distinguish between the two. However, the spectral intensity in the IR is much more distinctive and allows considerable information to be obtained about the two stems.
Spectra of artificial dyes and combinations thereof can often be difficult to distinguish from melanin in the visible range. However, the spectra can differ very markedly in the near infrared range.
The scattered light provides information about the condition of the fiber cuticle. An estimate of the radius of the fiber from the amount of refraction is also provided.
Light polarization improves SNR, possibly by excluding glare, and also improves detection of relative amounts of natural dyes and pigments.
Some embodiments of the present invention are further concerned with a method for predicting the result of a hair treatment operation using a predetermined prescription of the treatment composition (a predetermined composition).
The present embodiments consider the chemical dynamics of the process in which the hair is treated. The dynamics can be considered at two levels, the bleaching effects of oxidizing agents by reducing the initial concentrations of natural and artificial pigments and the interaction of the active agents with the hair. Separately, the spectrum finally reached is modified to take into account specular reflection.
The above prediction can be carried out based on data obtained from the optical reader, as will be explained in greater detail later herein.
ES 2 823 977 T3
The present embodiments comprise an apparatus method for predicting the result of hair treatment in a realistic manner. The system of using spectra instead of color coordinates is adapted but the chemical dynamics of the treatment operation are taken into account as are the effects of the final result of light scattering and specular reflection. The optical reader can provide data regarding light scattering and / or specular reflection.
Accordingly, the embodiments of the present invention are concerned with a method for predicting the result of a treatment operation using a predetermined composition recipe, which is carried out by measuring an initial spectrum of the hair being treated by obtaining sufficient characteristics of the fibers to make a real prediction of the result of a treatment; determining from the initial spectrum the presence and concentration of respective constituents; determine the reported concentration of the constituents following the bleaching effects of chemicals in the recipe, - determine the final concentrations of the constituents following the interaction of the chemicals with dyes in the fibers and from the final concentrations, predict a Final spectrum of the hair from which the color of the fibers can be calculated. While preferably all these features and actions should be carried out in some embodiments of the invention, fewer features may be sufficient for good prediction of results.
Embodiments of the present invention are concerned with a dispensing device that is configured to provide a hair treatment composition after determination of the chemical and physical characteristics of the keratinous fibers to be treated.
Embodiments of the present invention are concerned with a dispensing device that is configured to provide a composition for treating hair, after computationally selecting a composition that would impart a desired treatment of the hair.
Embodiments of the present invention are therefore concerned with systems and methods that use spectral means to determine the chemical and physical characteristics of the hair being treated, computational means to select the composition that would impart a desired treatment of the hair based on the determined characteristics of the hair. hair and a dispensing device to provide an appropriate (custom) composition based on computational means.
The present inventors have further designed and successfully prepared and implemented solid, rapidly disintegrating formulations in the form of tablets, particularly substantially spheroidal tablets (ie, beads), to impart the desired treatment (coloring) of the hair.
The present inventors have further designed and successfully implemented a dispensing device suitable for dispensing the tablets disclosed herein and any other tablets for treating hair. Such a dispenser may be in communication with one or both of an optical reader and computational means to determine an appropriate composition for treating the hair (a custom composition or treatment). Optionally, the dispensing device prepares a personalized composition or compositions in response to information received from the optical reader and / or computational means (as described herein). These compositions can be prepared automatically.
As used throughout, the term "hair" refers to all fibers comprising keratin structural proteins, including but not limited to hair, hair, wool, and silk. The fibers can be located in a living body, for example a person or animal, or a non-living body, for example a wig, hair piece, or other non-living hair aggregation. In some embodiments, the hairs are hair or in some embodiments, the fibers are human hair.
It will be noted that while some embodiments of the present invention are described in the context of hair, use of these embodiments in the context of any hair as described herein is also contemplated.
As used herein, hair treatment encompasses coloring, bleaching, and any other discoloration of the fibers.
Herein, coloration refers to the alteration of a color of a substrate (eg, hair) by introducing a colored substance to the substrate. Examples of colored substances include pigments and dyes. The term "coloration" is also referred to herein as "dyeing."
Herein, bleaching refers to the alteration of a color of a substrate (eg, hair) by reducing the amount of a colored substance (eg, a natural pigment) in the substrate.
It will be noted that while some embodiments of the present invention are described in the context of coloring and / or dyeing, the use of these embodiments in the context of any hair treatment as described in the
ES 2 823 977 T3 herein is also contemplated. Thus, coloring can be carried out, coloring and bleaching can be carried out, and only bleaching can be carried out.
Herein, the term personalized with respect to a treatment, composition, combination and other expressions is intended to describe modified or adjusted according to specifications and / or preference to obtain a desired end result (desired effect of the hair, for example, a desired hair color).
The systems:
Some embodiments of the present invention are concerned with systems that aim to provide an accurate coloring result when treating the hair while considering the chemical and physical properties of the fibers and the desired result to be obtained by the treatment.
In some embodiments, the systems are configured to provide a customized coloring composition for the hair of an individual subject.
Such systems may comprise one or more of:
an optical reader that measures the specular and / or scattered light of the hair being treated (eg hair);
a computer-implemented unit or means (also referred to herein as a computational unit or computational means) for predicting the result of hair treatment and / or for selecting a recipe for a composition to obtain a desired treatment;
a composition that is selected as appropriate to obtain a desired treatment of the hair or a useful formulation to prepare the same and a dispensing device to provide the selected composition or a selected formulation to prepare the composition or a selected kit to prepare the composition.
In some embodiments, the system further comprises a unit for operating some or all of the aforementioned units, preferably an optionally portable unit.
According to some embodiments of the present invention, there is provided a system comprising an optical reader and a computational unit as indicated hereinbefore that is suitable for use in accurately predicting the outcome of a hair treatment by a predetermined prescription. and / or to select an appropriate treatment composition to obtain a desired effect (personalized treatment).
In accordance with some embodiments of the present invention, there is provided a system comprising an optical reader, a computational unit, and a dispenser device as indicated hereinbefore that is suitable for use in selecting an appropriate treatment composition to obtain a desired effect (custom composition) and to provide the selected composition or agents to form the selected composition.
According to some embodiments of the present invention, there is provided a system comprising an optical reader, a computational unit, active agents Usable to prepare a selected composition for treating hair and a dispensing device as indicated hereinbefore which is suitable for use in selecting an appropriate treatment composition to obtain a desired effect and to provide the selected composition.
According to some embodiments of the present invention, there is provided a system comprising active agents Usable to prepare a composition for hair treatment and a dispensing device as set forth hereinbefore that is suitable for providing a selected (personalized) composition. to treat hair.
In any of these embodiments, a color measuring instrument comprising the optical reader can be used to establish the initial hair color.
In any of these embodiments, at least part of the active agents Usable to prepare a selected composition is in the form of solid tablet formulations.
In any of these embodiments, the dispenser is interfaced with the computational unit, the algorithm can determine amounts of tablets to be selected by the dispenser. The algorithm can take into account individual properties of the hair to be colored, as described herein.
According to some embodiments of the present invention, in any of the embodiments of a system as described herein, comprising an optical reader, the optical reader is as described herein. The optical reader, which is also referred to herein as a hair reader, is
ES 2 823 977 T3 described hereinafter with respect to Figures 32A-39C.
According to some embodiments, in any of the embodiments of a system as described herein that comprises the computational unit, the computational unit is as described herein (and is also referred to as computational means, unit or means computer implemented).
The computational unit and associated prediction algorithm are described herein with respect to Figures 18-31.
According to some embodiments, in any of the embodiments of a system as described herein comprising a composition for treating hair, the composition is formed from a solid formulation in the form of tablets as described herein.
According to some embodiments, in any of the embodiments of a system as described herein that comprises a dispensing device, the dispensing device is configured to deliver tablets, such as the dispensing device as described herein.
In some embodiments, in any of the systems as described herein that utilize a composition that is made, at least in part from solid formulation (s), into tablets, the system further comprises a dispenser that it is configured to deliver the solid formulation (s) in the form of tablets.
The dispensing device is described herein with respect to Figures 1-8 and 40-46. An exemplary system is illustrated in Figure 47.
In accordance with one aspect of some embodiments of the present invention, a system for effecting hair treatment is provided, the system comprising:
an optical device for measuring the initial spectrum of the hair;
a computer-implemented unit for predicting the result of performing a predetermined treatment (for example, the result obtained by lightening the hair with a predetermined coloring composition or recipe), the unit comprising:
a constituent estimation unit to determine from the initial spectrum the presence and concentration of respective constituents in the hair;
a kinetic chemical reaction modeling unit to (a) determine the modified concentration of the constituents following the bleaching effects of chemicals in the recipe and (b) determine the final concentrations of the constituents following the interaction of the chemical agents with colorants in the hair and a spectral prediction unit to use said final concentrations to predict the final spectrum of the hair;
a solid formulation in tablet form, the formulation comprises at least one active agent selected from the group consisting of a color-imparting agent, an oxidizing agent, an alkaline agent and being for use in preparing a composition to effect treatment and a dispensing device configured to deliver a predetermined combination of tablets and optionally a predetermined concentration and / or quantity of liquid media and which is interconnected with the implement unit taped by computer, wherein the pre-combination of the tablets is selected by the computer-implemented unit while the initial spectrum of the hair and the treatment to be carried out are considered.
In some embodiments, the solid formulation used in such a system further comprises a water-soluble super-disintegrating agent that optionally is such that it swells upon contact with an aqueous solution, as described herein.
In some embodiments, the composition useful to effect the desired treatment is a coloring composition as described herein.
In accordance with one aspect of some embodiments of the present invention, a system for effecting hair treatment is provided, the system comprising:
an optical device for measuring the initial spectrum of the hair, the optical device comprising:
a lighting unit to illuminate the hair;
a measuring unit comprising at least one sensor for optically measuring hair during
ES 2 823 977 T3 illumination by the illumination unit; wherein the sensor and a beam from the illumination unit respectively subtend a light diffusion angle in the hair that is measured, to thereby ensure that the sensor primarily measures light of the beam of illumination that is diffused or dispersed by the hair;
a computer-implemented unit to determine from the initial spectrum the presence and concentration of the respective constituents in the hair;
a composition comprising at least one active agent selected from the group consisting of a color-imparting agent, an oxidizing agent, a thickening agent, and an alkaline agent, the composition is such that the amount and concentration of each of the agents Active ingredients are selected to effect the treatment of the hair and a dispensing device is configured to provide the selected composition, the dispensing device is interconnected with the computer-implemented unit, wherein the predetermined amount of each of the active agents is selected by the computer-implemented unit while considering the initial spectrum of the hair and the desired treatment to be performed.
In accordance with one aspect of some embodiments of the present invention, a system for effecting hair treatment is provided, the system comprising:
an optical device for measuring the initial spectrum of the hair;
a computer-implemented unit to predict the final spectrum of the fibers following treatment with a selected composition and a mixer or dispenser to prepare the selected composition.
In some embodiments, such a system further comprises active agents as described herein to prepare the selected composition and in some embodiments, at least part of the active agents are in the form of tablets. In some of these embodiments, the dispensing device is configured to deliver selected amounts and types of tablets to provide the selected composition. In some of these embodiments, the dispenser is further configured to deliver selected amounts and concentrations of liquid media to be mixed with the tablets or any other form of active agents to provide the selected composition.
Methods:
In accordance with one aspect of some embodiments of the present invention, methods of treating hair are provided that are effected by performing one or more of the following:
analyze the hair to be treated;
computationally process the analysis of the fibers to be treated to select the components (active agents) and the concentration of each component in an appropriate composition to provide the desired treatment to the hair and optionally select a duration, speed and / or temperature for the application of each one of the components and / or the composition as a whole;
provide the selected (custom) composition and apply it to the hair.
The selected (custom) composition can be provided by mixing the components manually or by an automated dispenser.
The selected (customized) composition is advantageously prepared from solid formulations, in the form of tablets and more advantageously by fast disintegrating tablets as described herein. A suitable automated dispenser for dispensing tablets is advantageously used for this purpose.
Furthermore, according to one aspect of some embodiments of the present invention, there is provided a method for predicting the result of hair treatment (hair coloring operation) using a predetermined composition, the method comprising:
measure the initial spectrum of the hair;
determining from the initial spectrum the presence and concentration of the respective constituents;
determining the modified concentration of the constituents following the bleaching effects of the chemical effects in the composition;
determine the final concentrations of the constituents following the interaction of the chemical agents with dyes in the fibers and from the final concentrations, predict the final spectrum of the fibers from which the treatment of the fibers can be calculated.
ES 2 823 977 T3
Furthermore, according to one aspect of some embodiments of the present invention, there is provided a method for predicting the result of a hair treatment (eg hair coloring operation) using a predetermined composition (eg coloring recipe hair), comprising the method:
measure the initial spectrum of the hair;
from the final concentrations of natural factors of the fibers and of factors obtained from the predetermined composition, predict the final spectrum of the fibers after the treatment;
correct the final spectrum for specular reflection effects and further correct the final spectrum corrected for specular correction effects with an additional correction for light scattering effects.
Such methods may be combined with a hair treatment method to allow a subject to approve the desired result or otherwise modify it as desired prior to treatment, to allow the subject to determine the composition to be used or to allow the subject to practitioner select a personalized treatment according to the desired result.
Furthermore, in accordance with one aspect of some embodiments of the present invention, a method for obtaining optical measurements of hair (eg, hair) is provided, the method comprising:
applying a light source to the fibers;
optically measure the illumination of the fibers from a diffusion angle in relation to the illumination source, the illumination angle falls between 45 degrees and 135 degrees, to obtain by this a measurement whose main components are light that has been diffused or dispersed by the fibers of the light source.
Such a method can be combined with any of the methods described herein to optically measure the initial spectrum of the hair.
According to some embodiments of the present invention, in any of the embodiments of a method as described herein that comprises optical measurements of the hair or hair, the optical reader is as described herein.
According to some embodiments, in any of the embodiments of a method as described herein that comprises computational prediction, the prediction is as described herein.
According to some embodiments, in any of the embodiments of a system as described herein comprising a composition for treating hair, the composition is formed from a solid formulation in the form of tablets as described herein.
According to some embodiments, in any of the embodiments of a method as described herein that comprises providing a selected or predetermined composition, a dispenser device interconnected with a computational unit is used to provide at least part of the components of the selected custom composition. In some embodiments, the dispensing device is as described herein.
The following is a more detailed description of some embodiments of the methods and systems as described herein.
I. Hair treatment result prediction:
Reference is now made to Figure 18 which illustrates an exemplary method for predicting the result of a hair coloring operation using a predetermined hair coloring recipe (predetermined composition). T to the method can be used to predict the result of any treatment of any hair.
The term recipe is used herein to define a coloring composition with predetermined concentration of active agents such as coloring agents, alkaline agents, thickening agents and / or oxidizing agents, and / or with predetermined conditions for applying each of these. agents or the composition as a whole.
At S1, the method obtains an initial spectrum from the subject's hair, commonly using a spectrometer.
In S2, the method calculates, from the initial spectrum, initial concentrations of keratin, eumelanin and pheomelanin as well as the initial Sanderson coefficients, which include the reflected light of the surface component (both specular and diffuse) of the hair and estimation of the hair diameter and cuticle condition.
ES 2 823 977 T3
In S3, the method obtains factors regarding the recipe dyeing process in terms of alkaline agent concentration, oxidizing agent concentration, temperature, solution viscosity, hair diameter, cuticle condition, and exposure duration.
The factors are used in a chemical reaction kinetics equation to determine modified concentrations of keratin, eumelanin, pheomelanin, artificial pigments, and the modified values of the Saunderson coefficients. Damage to hair is also estimated.
In S4, the recipe is used to provide a concentration factor of the color-imparting agent (for example, dye substance) and the concentration of the color-imparting agent substance is used together with factors for the concentration of the alkaline agent, concentration of the oxidizing agent (e.g. hydrogen peroxide), temperature, viscosity, hair diameter, hair porosity and duration of exposure, in order to determine the final concentration of the artificial colorant in the hair.
In S5, the final concentrations of the artificial dye and keratin, eumelanin, pheomelanin, artificial pigments and the final values of the Saunderson coefficients are used together to predict a final hair spectrum, using a spectrum calculation process also as an estimate. damage to hair.
The final spectrum can be used as is, or it can be corrected for reflected light for surface reflectance effects (both specular and diffuse).
Similarly, initial spectrum analysis to determine the constituents that are present can be corrected for light reflected from surface effects (both specular and diffuse).
A way of approximating the reflectance spectrum by having the magnitudes of concentrations of each ingredient, as well as their absorption spectra and dispersion spectra, can make use of the Kubelka Munk formula.
Kubelka Munk's approximation is of the form:
Q-RW)<sup>2</sup> Σίί = 1 ^ · Λ · (λ)<sub>η</sub> «W SÍLl Cn 'where:
R (A) = The diffuse reflectance in wavelength;
Κ (λ)<sub>η</sub> = The absorption, in wavelength, of n <sup>th</sup> ingredient;
S (A)<sub>n</sub> = The dispersion, in wavelength, of n <sup>th</sup> ingredient; Y
C<sub>n</sub> = The concentration of n <sup>th</sup> Colorant.
The internally diffuse wavelength reflectance -R (A) - can be obtained from the Sanderson correction formula, as will be discussed in greater detail later herein.
Predicting the final spectrum at S5 may further comprise correcting for reflected light for surface reflection effects (both specular and diffuse).
Similarly, initial spectrum analysis to determine the constituents that are present can be corrected for reflected light for surface reflection effects (both specular and diffuse).
Correcting for reflected light for surface reflection effects (both specular and diffuse) may comprise considering an air-to-hair boundary and an outer hair-to-inner region boundary and the condition of the cuticles.
The correction may involve applying a Sanderson correction, for example a correction of the form, RW<sub>meas</sub> - to <sup>1</sup> 1 - F (A) „, - FW,„<sub>t</sub> + ^(2)<sub>βΛΪ</sub>Ρ (λ)<sub>ίπί</sub> - aF (A), „<sub>t</sub> + where:
ES 2 823 977 T3 λ = wavelength α = The relative portion of reflected light from the surface reflectance (both specular and diffuse) that propagates to the spectrometer detector;
R (A) = Reflectance corrected by Saunderson's formula;
F (A) ext = The external Fresnel reflectance (light reflected from the surface (both specular and diffuse)) of the external side of the hair;
F (A) ¡nt = The internal Fresnel reflectance between the inner medium of the hair and the boundary region of the hair.
As mentioned above, the reflectance corrected according to the Sanderson correction -R (A) - can be inserted to the Kubelka Munk approximation.
In S3 and S4, the final concentrations of keratin, eumelanin, pheomelanin, and artificial dye can be calculated using a chemical reaction kinetic equation.
Calculation of final concentrations can take into account intermediates that appear from such chemical reactions, as will be discussed in greater detail later in this document.
A mixing apparatus can mix a treatment composition according to the recipe when the final result (eg color) is approved. The mixing apparatus may be a manual mixer or an automated mixer, optionally in the form of an automated dispensing device, which is configured to provide the final calculated concentrations of each of the color imparting agent, the oxidizing agent and / or the alkaline agent and optionally a thickening agent, as will be further detailed hereinafter. When automated, the mixing device is preferably interfaced with the computer-implemented unit that executes the calculations described herein.
The implementation of the algorithm is now considered in greater detail. The method can be implemented by a computerized process that outputs the optimized prescription of hair treatments for a given initial hair (or any other hair) and a definition of the desired target treatment (eg coloring). The calculations use a priori knowledge of hair colorants in terms of their optical properties, as well as the evolution imposed, on the natural components in the hair, due to different hair treatments. Once these items are defined, given an initial hair coloring, the system considers a plurality of hair treatments. For each treatment, the system approximates the final result using physical and chemical formulas. Finally, the system chooses the treatment that best matches the target color (or any other treatment) while minimizing damage to the hair and the duration of treatment. It may be that the same person has several sites in the hair that require different measurements and different treatments, but with global considerations. For example, one can have a natural portion with natural coloring close to the scalp and hair roots and older hair away from the scalp that is already colored. The system acquires two measurements respectively and performs separate analysis for each part. However, the overall color of the head may take into account the color unit between the two portions, such that the choices for coloring in each portion are influenced by the overall appearance of the color unit.
The initial hair is measured with a spectrophotometer that includes at least the visible range. The units of the measured spectra are given in terms of relative reflectance, in the sense of the percentage of light that the hair reflects at each wavelength. Then, the relationship between the spectra and the concentrations of the components that comprise the hair are analyzed by the Kubelka Munk formula in the infinite thickness substance approximation, with the Saunderson correction formula. The reflectance measurement consists of two components: the internally diffuse reflectance and the light reflected from the surface component (both specular and diffuse). Diffuse reflectance involves scattering light in equal intensity for each solid angle in space, while light reflected from the surface includes both a specular portion that prevents light rays from traveling along specific sector boundaries and a diffuse portion, most of the cuticles. The internally diffuse component obeys the Kubelka Munk approximation while the light reflected from the surface (both specular and diffuse) is treated by the Sanderson correction formula.
Kubelka-Munk (in the approximation of substance of infinite thickness):
(l-fi (A))<sup>2</sup>
2'RW Z ^ iC<sub>n</sub>-sw<sub>n</sub>
ES 2 823 977 T3 where:
R (A) = The internally diffuse reflectance in wavelength.
Κ (λ)<sub>η</sub> = The absorption, in wavelength, of the nth ingredient.
S (A)<sub>n</sub> = The dispersion, in wavelength, of the nth ingredient.
C<sub>n</sub> = The concentration of the nth dye.
Saunderson correction:
As mentioned hereinabove, reflectance is assumed to consist of two types: an internally diffuse portion, obeying the Kubelka Munky formula, a surface reflected light portion (both specular and diffuse). Kubelka Munk's model does not take into account the light reflected from the surface (both specular and diffuse), which can be considered border effects. The light reflected from the surface (both specular and diffuse) is due to differences in the refractive index between the air boundary and between the internal environment in the hair and the condition of the cuticles. For example, differences in refractive index at the boundary between a hair sample and air give rise to a certain amount of specular reflection while small cuticles diffuse the light they reflect. The magnitude and angle at which this reflection is reflected depends on the luster of the sample, the structural geometry of the sample, and the optical setup of the spectrometer. The correction deals with two border effects, one on its external side (air-hair) and the other on its internal side (border region of the hair to the internal middle of the hair). The optical setup is also taken into account in order to describe the relative portion of specular reflection propagating towards the spectrometer sensor.
<sub>+</sub> ext W)
Isolating R (A) gives:
rs / ·] \ / rjíecij where:
A = wavelength a = The relative portion of reflected light from the surface reflectance (both specular and diffuse) that propagates to the spectrometer detector.
R (A) = Reflectance corrected by Saunderson's formula. This is actually the portion of reflectance that is due to diffuse behavior only.
F (A) ext = The external Fresnel reflectance of the external side of the hair (air-hair)
F (A) ¡nt = The internal Fresnel reflectance between the internal medium of the hair and the boundary (border of the hair to the internal medium of the hair).
Once R (A) is approximated by the Saunderson correction formula, it can be inserted into the Kubelka Munk formula.
Extraction of optical properties between natural hair:
The reflectance curve of natural hair is determined for the most part by the different ingredients it consists of. Each ingredient contributes its own absorption and dispersion curves in relation to its concentration. Once an illumination spectrum and a reflectance curve are given, the translation into color coordinates is trivial when using standard formulas such as CIE.
The optical properties of the ingredients can be calculated by analyzing spectra from different hair samples and taking samples from the natural hair space. The quantity of ingredients can be chosen arbitrarily during the analysis, as long as the number of equations is not so low that the number of variables. There are possibly many different ingredients in natural hair, however only some of these
ES 2 823 977 T3 significantly influence absorption and dispersion. Therefore, a decision regarding the maximum permissible error size in the optimization process serves to choose the number of ingredients in the hair. The lower the number of ingredients, the higher the calculation error and vice versa.
A choice of three different ingredients was found to introduce adjustments to measurements with low difference errors. These components are strongly correlated to the known natural components of hair: Keratin, Eumelanin and Pheomelanin. Keratin is what the hair envelope also does as internal fibers within the envelope. Eumelanin and Pheomelanin are two types of Melanin dye that provide a general class of natural pigments. Eumelanin is a dark brown pigment that is the most common pigment in most hair, while pheomelanin is generally present in moderate concentrations and contributes to the reddish-yellow tint.
Model for hair coloring:
The extraction of absorption and dispersion curves between the different hair ingredients requires the setting of an arbitrary positive non-zero constant value for one of the curves of one of the ingredients for all wavelengths, in order to obtain a set of nonhomogeneous equations with a finite set of solutions. For example, the Keratin dispersion curve can be chosen to be 1 for all wavelengths.
The hair coloring process refers to the insertion of dye colorants to the hair on the one hand and the reduction of initial melanin on the other hand. An experiment in which different samples of natural hair were exposed to the chemical compounds of the dyes, but in the absence of the colorants themselves, revealed spectra that spanned beyond the space of natural hair. Thus, using extended spectra you can reveal additional information around the dyes. A procedure based on the emergence of an additional dye, with concentration proportionally increased with the reduction of the Eumelanin concentration, proved to be robust and reliable.
The hair coloring process is mainly dominated by the concentrations of the dyes, temperature, concentration of the oxidizing agent (for example, hydrogen peroxide) and the percentage of ammonia, or other alkaline agent, which determines the pH level of the solution. . These magnitudes strongly influence the speed of reactions during hair coloring.
The reduction of Melanin during exposure to hair dyes is dependent on its initial concentration, the percentage of the alkaline agent, the percentage of the oxidizing agent, temperature, solution viscosity, hair porosity and duration of exposure. A functional relationship is characterized empirically from experiments as follows:
Cf = Melanin foinetics (Ci, Ca, Ch, T, t, v, p) where:
f Melanin kinetics = melanin kinetics function
Ci = Initial Melanin Concentration
Cf = Final Melanin Concentration
Ca = Concentration of alkaline agent in solution (for example, ammonia).
Ch = Concentration of the oxidizing agent (eg hydrogen peroxide).
T = Temperature t = duration (time of exposure to treatment) v = viscosity of the solution p = porosity of the hair
Melanin kinetic function increases monotonically with increasing temperature (T), alkaline concentration (Ca), oxidizing agent concentration (Ch), duration (t) and hair porosity (p). The function decreases monotonically with increasing viscosity (v).
The function coefficients are optimized to display best-fit results between spectral predictions and spectral measurements at different values of known parameters.
ES 2 823 977 T3
Different kinetic functions apply to Eumelamna and Feomelanma.
Alternatively, no analytical function is introduced, but instead an empirical grid of fitted measurements provided with a plurality of different values over all dimensions. The prediction of Ct is then estimated by means of KNN (averaging of k nearest neighbors on the grid) or standard interpolations.
Summarizing the aforementioned arguments to a mathematical formulation it is obtained, for given natural hair spectra:
_ (1 + Ceu, í '^ Eu + ^ Pheo.i' ^ Pheo 'Rj 1 + C<sub>Eud</sub> S<sub>Eu</sub> + Cph<sub>eo</sub> j S<sub>phso</sub>
Where R, means the initial reflectance after correction by the Saunderson formula.
For example:
After prescription dyeing of N specific hair dyes the final spectra can be predicted as follows:
í ^ \ _ ^ ker * ^ Eu. / '^ Eu + Cpheo.f' kpheo + (CeuT <sup>—</sup> ^ Eu. /) '^ Adder + Ση = 1' Λ (Όη + C<sub>Eu</sub>j 'S<sub>£ u</sub> + Cp} i<sub>eo</sub>f 'Spfteo + (Cffíu <sup>—</sup> ^ E-uf) '^ Adder Ση = 1
Then, a first spectral prediction is calculated by the Kubelka Munk equation:
fK \ Í<sup>K</sup>\<sup>2</sup> i<sup>K</sup>\ <sup>r</sup>Prea <sup>1 +</sup> (t) ". (τ ') <sup>+ 2</sup>'E / \ O Jp<sub>re</sub>And p<sub>net</sub> f Pred
And the final fit of a hair spectrum is available by considering the optimized Saunderson coefficients, a, Fext and F¡nt for the final spectra:
p, (<sup>1</sup> “ 1 <sup>—</sup> δ nr) 'fprtd setting = π + ------- _ --------------- 1 bní' ^ Pred
The magnitudes of the kinetic coefficients ai, 02, as, 04 and the absorption curves of the dyes: Κι, K2, Ks ... Kn and dispersion Si, S2 ,. . . Sn are optimized by processing multiple hair measurements, before and after coloring with known recipes and with appropriate statistical sampling. Optimization seeks to minimize the sum of the spectral squared differences.
Once a reflectance spectrum is measured or predicted it can be translated into color coordinates under a chosen desired ambient radiance spectrum. The translation follows the standard CIE color space. The translation of spectra to color coordinates is familiar to those dealing with the art of spectral measurements and colors.
The distance between the color coordinates of the object and the target can be given by a vector distance:
2 2
ColorDistance- ^ dE = ^ (X<sub>Qobject</sub> - X) + (¾ ^ ~ Y<sub>Diana</sub> ) + (, Z<sub>objection</sub> ~ Z<sub>Diana</sub>}
Reference is now made to Figure 19 which is a simplified graph illustrating the kinetics of Eumelanin concentration versus the rate of the alkaline agent (eg ammonia). The duration, the oxidizing agent and the temperature were kept constant.
Reference is now made to Figure 20 which is a simplified graph showing the kinetics of Eumelanin concentration versus the rate of the oxidizing agent (eg, hydrogen peroxide). The rate of the alkalizing agent (eg ammonia), duration and temperature were kept constant.
Reference is now made to Figure 21 which is a simplified graph showing the concentration kinetics
Eumelanin ES 2 823 977 T3 versus duration of exposure. The alkalizing agent ratio (eg ammonia), oxidizing agent ratio (eg hydrogen peroxide) and the temperature were kept constant.
Reference is now made to Figure 22, which is a simplified graph in which the green curve was better adjusted to the measurement of the natural hair spectra by optimizing the Eumelanin concentration and Pheomelanin concentration in the Kubelka Munk formula and the coefficients of Saunderson.
Reference is made herein to Figure 23 which is a simplified graph in which the green curve is the fit curves calculated by the Kubelka Munk and Saunderson formula for coloring natural hair with a known dye recipe looking for adjust the measurement curve in red.
Reference is now made to Figure 24 which is a simplified graph illustrating the distribution of spectral squared differences after optimization. The optimization process seeks to minimize the sum of the squared spectral difference between predictions to measurements by using the model coefficients.
Reference is now made to Figure 25 which is a simplified graph showing the optimization of coefficients for a model to minimize the overall sum of spectral squared differences between a measured set of 666 hair samples. Then a statistical distribution of the color difference is calculated.
An algorithm for predicting the coloration of initially colored hair requires that a measurement be taken from the initially colored hair. In a first alternative, the estimation of the dyes is done using an IR signal.
The signal in the IR range around 950 nm is sensitive to the existence of melanin and very indifferent to dyes. Consequently, the concentration of the natural hair ingredients can be extracted by analyzing the signal in the IR region.
In initially colored hair the components inside are natural hair ingredients and unknown colorants with unknown concentrations. Accordingly, an approximation is made to estimate the initial concentrations of each natural hair ingredient according to the IR region and to assign the residual absorption or residual dispersion to the colorants in the hair.
In the first stage an estimate of N natural hair ingredients are extracted using the best fit (least squares optimization) the concentration of each ingredient to the measurement in the IR:
<img file="ES2823977T3_D0001.tif" />
ΣΑιC „, / K \ _ (1 —r)<sup>2</sup>
Then, the residues are defined as follows for the entire region of the spectra:
<img file="ES2823977T3_D0002.tif" />
(i ~ O<sup>2</sup> r
ίΣη = ι + h<sub>Beef</sub>
VN C í
ΣιΥ r ·, v η = 1 <sup>υ</sup>η.ί <sup>Λ</sup>η <Σπ = 1 Qi.t ' <sup>+</sup> $ Res
<img file="ES2823977T3_D0003.tif" />
The magnitude is related to the reflectance after the Saunderson correction and the calculations are processed for each wavelength increment separately.
The prediction of the final spectra for the initially colored hair, with respect to the recipe of N dyes is then formulated as follows:
(Κ \ Σί ^ -K „+ f · K<sub>Beef</sub> + Σ ^ ι C<sub>n</sub> KW „
Ύ, ο Σϊ<sub>=1</sub> c<sub>n</sub>.<sub>F</sub> Κ „+ [· s<sub>Beef</sub> + ςϊ<sub>=1</sub> c „· s (A)<sub>n</sub>
Where f means a scalar from 0 to 1.
The relationship between the final concentration of the natural hair ingredients is given by the kinetic formula.
As in the case of natural hair, the magnitudes of the residual coefficient f, the kinetic coefficients and the curves 29
ES 2 823 977 T3 of absorption dyes: Ki, K2, ..., Kn and dispersion Si, S2, .., Sn are optimized by processing multiple measurements of the hair, before and after coloring with known recipes.
Reference is now made to Figure 26, which is a simplified graph illustrating the optimization of the coefficients of a model for initially colored hair to minimize the overall sum of spectral squared differences between a set of 666 measured hair samples. After this, a statistical distribution of the color difference can be calculated.
Reference is now made to Figure 27, which is a simplified graph showing the kinetics of Eumelanin concentration versus ammonia, for fixed hydrogen peroxide and duration.
Reference is now made to Figure 28, which is a simplified graph showing the kinetics of final Eumelanin concentration versus% Ammonia concentration in the case of an initially colored hair model. The duration and concentration of hydrogen peroxide were kept constant.
Reference is now made to Figure 29, which is a simplified graph showing the kinetics of Eumelanin concentration versus Hydrogen Peroxide concentration. Ammonia concentration and durations were kept constant.
Reference is now made to Figure 30, which is a simplified graph showing the kinetics of Eumelanin concentration versus duration. The concentration of Ammonia and Hydrogen Peroxide were kept constant.
Reference is now made to Figure 31 which is a simplified flow chart showing a process to obtain the coloring factors of natural hair and to obtain ingredients and factors concerning ingredients for products generally used in treatment recipes for hair. hair.
Obtaining a model for natural hair coloring:
In the above, it has been assumed that the factors are known about substances in the recipes and that the natural hair factors and other hair factors can be derived from the measured hair spectrum. The following is a summary of a system for coloring natural hair according to the algorithms discussed above that provide the data required by the algorithms.
1. Natural hair ingredients:
In step S6, the process analyzes the spectra of a plurality of natural hair that cover the entire space of natural hair of all colors according to Figure 13.
to. Number of ingredients. Finding how many ingredients are required for the best fit of the measurement spectra under the assumptions of Kubelka Munk and the Saunderson correction - the value of M. The values are then adjusted to initial values in step S7. In step S8, the K and M values are optimized for all M ingredients.
In step S9, optimizations are carried out for each spectrum. In step S10, a fit quality is determined which is compared with a threshold in step S11. The solutions are stored in step S12.
b. Save Kubelka Munk coefficients. This stage maintains the coefficients of K (absorption) and S (dispersion) for each ingredient.
two. Melanin kinetics:
to. Experiment. An experiment is prepared in which multiple natural hairs that cover the entire space of natural hair of all colors are exposed to the materials in the dyes but without the colorants themselves. The treatment includes different durations, temperatures, concentrations of the alkaline agent, viscosities and concentrations of the oxidizing agent. All spectra of all hair are measured in the experiment outlined above before treatment and after treatment.
b. New ingredients are defined that appear as bleaching by-products. The data are analyzed in order to extract the emergence of new ingredients within bleached hair and their K (absorption) and S (dispersion) are calculated as well as their concentrations among bleached hair.
c. Kinetic functions are extracted. The data are analyzed in order to define the functions that relate the final concentration of each ingredient to its initial concentration, with respect to parameters such as temperature, viscosity, pH level, duration, hair diameter, hair cuticle condition and concentration
ES 2 823 977 T3 of oxidizing agent. The functions can be purely empirical or they can obey diffusion and reaction rate formulations with appropriate optimized coefficients.
3. Dye kinetics and optical properties:
to. Experiment. An experiment is prepared in which multiple natural hairs that cover the entire space of natural hair of all colors are colored with all dyes and their mixtures. Hair coloring can include two classes of coloring agents. One of them is a direct dye that already carries color and migrates as it is to the hair, while the other agents are different dye precursors and dye couplers that migrate to the hair and then interact chemically with the mediation of oxidizing agents and alkaline agents. , to produce dye molecules in the hair. The treatment includes different concentrations of dye, viscosities, durations, temperatures, concentrations of alkaline agents and concentrations of oxidizing agents.
All hair spectra are measured before treatment and after treatment.
b. Optical properties of the dyes are defined. The optical properties of the dyes are extracted in terms of their k and s values. Care is taken to include all possible combinations that can be produced during the development of the colorants.
c. Extract kinetic functions. The data are analyzed in order to define the functions that relate the final concentration of each colorant with its initial concentration or the concentrations and reactivity of the different dye precursors and dye couplers that were combined to introduce them to the solution, with respect to parameters such as temperature, solution viscosity, alkaline agent concentration, duration, hair diameter, hair cuticle condition and oxidizing agent concentration:
<sup>C</sup> heating agent = (C ^ C¿, C<sub>p</sub>, T<sub>r</sub> t, V, p) = f<sub>m</sub>{c<sub>TO</sub>, C<sub>r</sub>, T, t, v, p, ..... C<sub>prJ</sub>, C<sub>Coplsdl¡r</sub>_......
Where:
V, P) kinetic function of n <sup>th</sup> direct dye
F <sup>V</sup>'P' Ll '' kinetic function of m <sup>th</sup> Colorant
C, = initial direct dye concentration
Ccoiorant = final direct dye concentration
Ccoiorante_m = final dye concentration, reactant interaction product
C Γ pr ^ '-' pr_i concentrations of dye precursors c --c coupler '^ coupler _j concentrations of j dye couplers
Ca = Concentration of alkaline agent in solution (for example, ammonia).
Ch - Concentration of the oxidizing agent (eg hydrogen peroxide).
T = temperature
ES 2 823 977 T3 t = duration (time of exposure to treatment) v = viscosity of the solution p = porosity of the hair.
The functions can be purely empirical, or they could obey reaction rate and diffusion formulas with appropriate optimized coefficients.
Alternatively to that, no analytical function is introduced, but instead, an empirical measurement set grid is provided for a plurality of different values over all dimensions. The prediction of Ccolorante and Ccolorante_m, is then estimated by means of KNN (averaging of k closest neighbors on the grid) or standard interpolations.
II. Optic reader
In accordance with one aspect of some embodiments of the present invention, an optical reader is provided that measures sufficient characteristics of the hair to make a realistic prediction of the outcome of a hair treatment operation, as defined herein (for example, hair coloring, such as hair).
Referring now to the figures, Figure 32A illustrates a device 10 for the optical measurement of hair (eg hair), comprising an illumination unit 12 for illuminating the hair 14.
Measurement unit 16 (not shown in Figure 32A includes an optical collection system for optically measuring hair during illumination by the illumination unit. The optical collection system and a beam of the lighting unit respectively subtend a light diffusion angle of between 45 degrees and 135 degrees on the hair that is measured and thus ensures that the sensor mainly measures the light that is scattered or scattered by hair, as opposed to direct reflection from the outer side of the cuticle or cuticle-cortex interface (Fresnel reflection). In other words, the beam of illumination is incident on the hair and a resulting beam of diffuse light is collected at an angle of 4-5 to 135 relative to the beam of illumination.
In Figure 32A the lighting unit is positioned to illuminate said hair from an azimuth elevation and the sensor is positioned perpendicular to the hair. The lighting unit may include multiple lighting sources configured respectively to illuminate said hair from a plurality of substantially azimuth angles around the hair.
In Figure 32B the opposite configuration is used and the measurement unit comprises a plurality of sensors positioned around the hair at an azimuth elevation. The lighting unit is placed perpendicular to the plane of the hair. In both of the above configurations, multiple lighting angles as well as pick-up angles can be used. A third configuration could also be beneficial, in which neither the lighting nor the pick-up is perpendicular to the hair, such a configuration is used in, for example 135 degrees.
Another possible geometry is illumination and harvesting from the same direction, for example approximately perpendicular to the hair, when using an optical beam splitter (for example 50:50) or a polarizing beam splitter. In the latter possibility, the specular component of the reflection is also removed by choosing the cross-polarization configuration.
The illumination unit may include two substantially opposite illumination directions facing each other along an axis of the hair. A measurement is made for each direction and the difference in measurement results provides an indication of the condition of the hair cuticle, as will be described in greater detail later herein.
The lighting unit can use light sources that are actually or substantially parallel to the axis of the hair, albeit from respectively different azimuth angles around the hair.
The light sources can illuminate the hair at different times. The temporary window formation in the sensor allows the illumination of the different sources to be measured separately. Alternatively, the light sources can illuminate different regions of the inspected hair. The spatial solution in the sensor allows the illumination of the different sources to be measured separately.
The lighting unit may include a main broadband lighting source and subsidiary lighting sources. Processing electronics can use differential illumination results by comparing different sources in order to obtain particular kinds of information such as the angle of the hair in relation to any source of illumination.
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The processing electronics can then use the angle of the hair to correct a spectrum of hair for the different lighting angle.
Processing electronics can additionally use differential illumination results to distinguish between specular and diffuse reflected light from the hair, each of which gives different information about the hair.
The main light source can be used for spectroscopy and the subsidiary light sources can use either spectroscopy or angle measurement.
There may be four sources of illumination, each at the same elevation angle relative to a plane perpendicular to the detection axis, as will be discussed in greater detail later herein. In one example, the azimuth angle with respect to the axis of the hair is 30 ° for two of the four light sources and 150 ° for a third and a fourth of the light sources.
The sensor can detect the visible, near ultraviolet, ultraviolet, near infrared and infrared parts of the electromagnetic spectrum. As explained, a global spectrum that covers the visible, infrared and near infrared parts of the spectrum contains information that allows melanin-based hair factors to be distinguished. For very dark hair, the vast majority of the data required to calculate melanin concentration is in the NIR and IR. The visible part of the contrast spectrum allows to define the hair color in any color space such as laboratory or others, but does not allow the calculation of the melanin concentration.
Typical sensitivity ranges are the 350-1,500 nm wavelength range or the 350 - 750 nm wavelength range, or the 400-950 nm wavelength range.
As discussed in greater detail hereinafter, the sensor may include one or more calibration regions that receive direct calibration light from the optical elements that has not been reflected by the hair. The calibration light allows the sensor to be calibrated.
A polarizing element, for example a controllable polarizing element, can be inserted at various locations in the optical system.
As discussed hereinafter, hair clips can be provided to hold hair in position for measurement.
In service, the optical device can apply a light source to the hair, then optically measure the illumination from a diffusion angle that commonly falls between 45 degrees and 135 degrees. The use of the angle is to obtain a measurement whose main components are light that has been scattered or scattered by the hair, as opposed to direct reflection.
The optical reader is an optionally portable tool that measures the optical characteristics of hair (or any hair). The calculation of the properties of the hair can be done outside the optical reader, for example in the computational unit. The parameters can be used to plan a hair coloring procedure or any other hair treatment operation (eg coloring, bleaching) and estimate the actual hair color after the operation.
Various optical data can be measured, such as the absorbance spectrum, a specular reflectance spectrum or a spectrum of light scattered or scattered by hair or combinations thereof. Also, polarization characteristics or fluorescence characteristics can be measured.
Calculated hair properties can include hair color in the visible range and relative amounts of melanin in the hair, relative amounts of Eumelanin, relative amounts of Pheomelanin, and relative amounts of both Eumelanin and Pheomelanin together, as well as relative amounts of the hair dyes. hair to hair, including total dye amounts and amounts of specific dye components.
Other calculations can be related to the relative amount of water in the hair; and a relative extent of hair elements that affect dyeing kinetics, such as cuticle condition (degree of opening), hair radius, etc., as will be explained in greater detail later herein.
The optical reader is designed to measure any hair and any hair substitute, where the hair and its substitute can be human hair (natural or colored), animal hair (natural or dyed), any kind of hair substitute or artificial hair , including wig hair, creatinine fibers, costume hair, etc .; and hair manufactured for hair catalogs.
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The hair is not limited to the hair of the head or its substitute but to the hair of any part of the body and its substitutes.
Opto-Mechanical Lighting:
As discussed with respect to Figure 32A above, the optical reader comprises two modules, a lighting module and a detection module, (among other modules, such as calculation, communication, etc.).
Lighting Module:
An exemplary lighting module contains four LEDs in the following wavelength range:
I: Monochromatic or narrow bands 400 (390 - 410 nm)
II: white or visible (430 - 750 nm)
III: Monochromatic or narrow band 850 (820 - 880 nm)
IV: Monochromatic or narrow band 950 (920 - 980 nm)
The embodiment may use different LEDs or other light sources that illuminate different wavelength bands.
A variant can use fewer LEDs or more LEDs, for example an additional LED that illuminates in the 750-820 nm band and can be provided to fill the space between the second and third LEDs in the list above.
LED lighting can be carried out differently from simultaneously. Illumination for spectroscopy purposes can use an illumination intensity level range that is less than 1: 2 (the ratio between maximum and minimum illumination levels) in order not to obtain a mixture of different wavelengths in one area. of hair measure.
The following lighting programs can be used:
- each LED lights at a different time.
- The first 2 LEDs (I, II) light up at one time and the others (III, IV) at the next time.
Lighting programs can be used to build duty cycles for LEDs.
LEDs can be mounted in a small package such as ACULED produced by Perkin Elmer. This packaging allows a very small distance between the different LEDs, such that the lighting hitting the hair of each LED will be almost at the same angle given that a Kohler-like lighting optical component is used.
Illumination from LEDs is advanced through a lens and can hit the hair at a typical 45 ° angle. Note that other angles can be used as desired.
The lighting module can be designed to be directional. Specifically, the light is directed azimuthally to be parallel to the hair. The idea of directionality is in order to allow viewing only of diffuse light. Illumination from wide NA or other azimuth angles are prone to mixing specular and diffuse light together.
Detection Module:
The detection module measures the light scattered from the hair (or any hair). The intention is that the measurement should separate the effects of at least one of the following: diffuse reflection from the fiber cortex, specular reflection of any kind, and absorption.
Reference is now made to Figure 32C which is a simplified diagram illustrating one possible embodiment of an optical system suitable for detection. The illumination from the LEDs, which is scattered by the hair 100, passes through a cylindrical lens 110 and a narrow slit 120. After the slit, the light passes through a small aperture, in the example a 3-hole diameter aperture. , 2mm, 130 and an additional lens 140. Wavelength separation is carried out using grating 150.
Light from grating 150 is deflected using a mirror 160 and collected using a three lens collecting optical component 170 onto a sensor 180.
In the sensor, the light of different wavelengths falls in different columns, due to the effect of the grating 150, thus obtaining a full spectrum.
Reference is now made to Figures 33A and 33B which are respectively schematic block diagrams showing
ES 2 823 977 T3 show in greater detail the illumination angles and gathering angles in light in relation to the hair being measured. The main axis of the optical components is perpendicular to the hair and lies in the same plane defined by the hair and by the angle of illumination. The main lighting is a wide band lighting that illuminates the hair at an oblique elevation angle with narrow NA. The collection optics collect the scattered illumination above the hair in order to create the spectral data.
The detector may for example be a 180 two-dimensional CMOS / CCD sensor with a resolution of 1240 * 1080 such as Aptina MTM9001C125STM. The sensor can detect light in a range of 400 to 1,000 nm or wider, thus observing the full spectrum of illumination.
In Figure 33A, the light collection is perpendicular to the hair, thus capturing the scattered light. In Figure 33B, the light collection is at an oblique angle. Figure 33C shows the illumination and light collection from above.
Broad Spectrum Usage:
The optical reader creates a spectrum of the hair in a wide range of wavelengths, including the IR region, for example between 400 nm to 950 nm, but can be even broader, such as between 380 nm and 1,500 nm.
This spectrum can be obtained by using lighting sources such as:
- a combination of one or more LEDs, as described for the lighting module;
- a combination of several monochromatic lasers at wavelengths distributed over the interval;
- flash lamps such as Xenon lamps;
- Tunable lasers, -
- white lasers; or
- lasers with non-linear elements that split the laser illumination to multiple wavelengths or extend the wavelength to a broad band spectrum.
One of the main data relevant to recommending a hair treatment procedure (eg coloring) is the relative amount of melanin in the hair. In the current embodiment, the relative amount of melanin in the hair is found by adjusting the spectrum of the hair to the spectrum of melanin. To find the relative amount of both types of melanin, a linear function of both spectra is used in the adjustment process.
As explained above, melanin has strong absorption at the visible wavelength. Consequently, it is difficult to determine the relative amount of it, especially in dark hair, using only visible data. The IR spectrum is used to overcome this problem. In the tuning fixture, the spectrum of the IR region is used alone or with a higher weight than the shorter wavelength part of the spectrum.
Another parameter for hair treatment is the relative amount of hair dyes that remain from previous hair coloring treatments or other procedures. The spectrum of hair dye appears mainly in the visible region and is masked by the spectrum of melanin. Therefore, as soon as the relative amount of melanin is known, the melanin can be subtracted from the measured spectrum to reveal the spectrum of hair dyes.
The spectrum next to melanin subtraction can be used to estimate the relative amount of dyes in the hair and even relative amounts of each dye component.
The IR range contribution to calculate the relative amount of melanin starts at 750 nm and even at shorter wavelengths. Accordingly, working embodiments can usefully use any spectral range as long as the approximate 750 nm region is included.
Reference is now made to Figure 36 which is a simplified graph showing two typical hair spectra as percentages of reflection in the range 350-1550 nm. The solid broad line represents a spectrum of hair initially of a light shade and the dashed thin line represents a spectrum of hair after coloring and that is of a darker shade.
In the IR part of the range - the longer wavelengths - the spectrum of colored hair - dashed line - shows more reflectance, which means that the relative amount of melanin is lower. The low level of melanin is an effect of the dyeing procedure. The spectrum in the visible part of the range, which shows less reflected light, means that the pigments are absorbed into the hair.
What Figure 36 shows is that looking at a wide wavelength region that includes visible and near IR provides an advantage in being able to detect relative amounts of both melanin and hair dye.
ES 2 823 977 T3
Also looking at the IR, near 1,500 nm, the relative amount of water in the hair can be estimated, since water has a strong absorption near this wavelength.
The relative amount of water in the hair can affect the hair treatment process. For example, the dyeing kinetics of wet hair is different from that of dry hair. It is therefore also advantageous to observe the spectrum up to 1,500 nm or even beyond.
The above has explained how to detect relative amounts of melanin, dye color or water, when looking at a graph and a curve fitting algorithm has also been mentioned. It will be understood that there are also other algorithms to allow automated determination of such relative amounts from the spectra.
For example, the spectrum of known hair dyes can also be used in a curve fitting algorithm and the various possible algorithms can use the entire spectrum, specific points within the spectrum, or even one point on the spectrum to generate their findings.
The optical reader is not limited to using only the visible and near IR wavelength ranges. Any optical range can be used, such as a combination of one or more of UV, visible, near IR, mid IR, and far IR.
Illumination:
The optical reader can contain multiple light sources located at different angles to the hair (or other hair being treated). These sources can be used in order to improve the quality of the measured data by gathering more hair parameters in order to better estimate the dyeing kinetics that are used to plan a dyeing procedure. In addition, the hair reader can provide an estimate value of the angle between the hair and the hair reader to correct the measured data using the estimated angle.
Referring again to Figure 33A and the main lighting is a wide band lighting that illuminates the hair at an oblique elevation angle with a limited NA. The collection optics collect the scattered illumination above the hair in order to create the spectral data.
Hair cuticle search:
Reference is now made to Figure 33B which is a schematic diagram showing the illumination of the hair from two opposite directions of oblique lifting and light gathering to a perpendicular of the hair on the illumination side. The first broadband illumination is from an oblique elevation angle as in Figure 33A. Another beam of illumination strikes the hair in the opposite direction to azimuth but at the same elevation angle. The scattered illumination of the second direction differs from that of the main illumination since the hair cuticle is not symmetrical. The cuticle scatters the lighting from one direction differently from that in the opposite direction. The difference between the dispersion intensity strongly depends on the degree of opening of the cuticle. Figure 35A shows hair with a noticeable cuticle where high intensity scattering is expected for illumination from the right side and low intensity scattering from the left side. In Figure 35B in contrast, the cuticle is smooth and the spread on the two sides would typically be the same.
Accordingly, the difference between the amount of scattering measured from the main and opposite illumination directions can be used to estimate the degree of cuticle opening. This degree of opening affects the kinetics of the hair. Since the cuticle is more open, the dye enters the hair more quickly.
It will be noted that the second light source may be at other angles and elevations, for example not 180 degrees azimuth to the main source and not at the same elevation angle. Any angle is satisfactory if the proportion between the dispersion of the two sources can be used to estimate the opening of the cuticle.
Hair Radius:
Perpendicular lighting can be used to estimate the radius of the hair, which is also a relevant parameter for dyeing kinetics.
As the radius of the hair increases, the reflected illumination from a perpendicular light source increases.
The angle of the radius measurement source does not have to be precisely 90 degrees azimuth to the main source and not at the same elevation angle. Any angle is satisfactory if the returned lighting can be used to estimate the radius of the hair.
ES 2 823 977 T3
Angle Measurement and Correction:
Spectral data can have a strong dependence on the angle between the hair and the optical components of the system, that is, between the hair and the illumination and detection modules.
In the optical reader, most of the measured energy comes from scattering light from the body and hair surface rather than specular reflected light from the surface. Specular reflection has only a small effect on the relevant measured data (visual hair color, relative amount of melanin, etc.).
Using a different illumination angle (either elevation or azimuth) can result in more specular reflected light entering the spectral data.
Reference is now made to Figure 37, which is a simplified graph illustrating the measured reflectance powers of blonde hair at different measurement angles. Three different graphs are shown, solid line for the 400-700 nm wavelength range, dashed for the 700-900 nm wavelength range, and dotted for the full 400-900 nm wavelength range. As would be expected, 90 and 270 degrees, the different perpendiculars give maximum reflections and 0 and 180 degrees, the different parallel, give minimum reflections.
One embodiment uses multiple light sources at different angles relative to the optical components of the system in order to measure the angle of the hair and to correct the spectral data thereof.
Reference is now made to Figure 34A, which is a simplified side view of a hair reader 400 in accordance with one embodiment of the present invention. Figure 34B is a top view thereof.
The collection optics 402 are located perpendicular to the hair 404. Four light sources, preferably LEDs (A, B, C and D) illuminate the hair at the azimuth angle of (30 °, 150 °, 210 ° and 330 ° in relation to the hair shaft). These sources illuminate one at a time in order to allow separation of their signals at the sensor.
In the nominal case with the hair positioned correctly with respect to the optical components, the light collected from each light source should be the same, except for the cuticle effect, which is measured using opposing lighting.
If the hair has the wrong azimuth angle, the light returned from source A is different from B and the light returned from source C is different from D. Also, if the hair has the wrong elevation angle, the light returned from source A is different from C and the light returned from source B is different from D. However, using calibrated data, the angle of the hair can be estimated from the ratio of the four sources. As long as the angle is reasonable, the spectral data can be corrected.
If the angle is too large, the operator can be informed of a measurement error and given the opportunity to rearrange the reader or hair.
One way to correct the data may involve using calibrated data. The calibrated data may contain a spectral shift concerning different angles of illumination and azimuth. The data may consist of full spectra at different angles or coefficients for linear, parabolic, polynomial, or other estimated functions.
The calibrated data can be for a nominal hair or for each hair type or hair color as long as it can be learned from the uncorrected data.
Figure 34A illustrates four lighting sources. However, instead of using four light sources, fewer sources can be used.
In one embodiment, three sources A, B, and C are used and full functionality is nonetheless retained, since all concerning changes with azimuth and elevation angle still affect the sources in pairs.
One or more of the sources may be the sources used to measure the radius of the cuticle or hair.
Only two sources need to be used to estimate only azimuth (for example A and B) or only elevation (for example A and C).
In another embodiment, instead of multiple light sources, the angle of the hair can be measured using one light source and multiple light detectors. Such an embodiment has the advantage of not requiring light tilting.
A further embodiment uses a single sensor that angularly resolves the collected light.
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A further embodiment involves a combination of multiple sources and multiple detectors.
The light sources may be at other azimuth angles than described. The elevation angle is not restricted or fixed but can vary for each source or group of sources.
In a further embodiment, instead of using four or fewer lighting sources as discussed above, more sources can be used. Using more sources provides the advantage of using a more accurate angle estimate.
Lighting Sources:
The light sources can be activated in a sequential order in time where each source illuminates the hair at a different time. Thus, the scattered light for each source is easily separated by collecting the reflected light from each source at a specific time gate.
In one embodiment, the time difference between activation of each source is around 1/10 second, since it matches the actual frame rate of the sensor. Therefore if a set of nine LEDs is used there is about 1 measurement per second. In one embodiment there is a main illumination that contains 4 LEDs, an opposing illumination that is a single LED, and the four surrounding LEDs A'-D 'making a set of nine.
The opposing lighting and the four surrounding LEDs can in practice be any kind of lighting, LEDs, group of LEDs, lasers, lamps including flash lamps, etc.
Illumination sources can be narrow band to give only total energy data or they can be wide band to give full spectral data or partial spectral data.
Preferred Flow:
The sensor can obtain many images in a short time and thus multiple measurements can be made. The user can scan the hair using the hair reader and obtain data from multiple points along the hair.
A two-dimensional sensor can also allow in situ calibration using two lateral areas with specific calibration targets, to cover two dynamic ranges. The same can alternatively be obtained with a sensor, for example by electromechanical or electro-optical tilting.
Thus, a hair can be scanned from the root of the hair to the edge of the hair. The characteristics of the hair and consequently the required dyeing procedure and / or the resulting color can be calculated for different portions on the hair, which may have different characteristics.
For each scan point, the LEDs illuminate according to a predetermined sequence. The sequence can be for example:
* 400nm LED (from ACULED) * Warm white LED (from ACULED) * 850nm LED (from ACULED) * 950nm LED (from ACULED) * Opposite direction LED (optional) * Perpendicular direction LED * LED A * LED B * LED C * LED D
When each LED illuminates, the relevant part of the sensor, depending on the wavelength, is sampled by the electronic components of the hair reader.
The data from each LED can be analyzed in real time. If real-time analysis detects inappropriate reading data from a given LED (for example, too low or too high of a reading), the illumination of that LED can be repeated.
The data from a scan point can be used to analyze a previous point or a next point. For example, the signal from the opposite direction LEDs or AD LEDs can be averaged from multiple points to obtain more accurate data.
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Mechanical design:
Reference is now made to Figure 38, which is a simplified schematic diagram illustrating mechanical design elements of an embodiment of a hair reader in accordance with the present invention.
The mechanical elements can be designed to the hair reader in order to obtain better hair spectroscopy signals. Optical reader 300 contains two clips 190 near an optical component window 188. The clips direct the hair to be parallel to the lighting, thus enhancing the signal.
Instead of bras, anything that directs the hair in the right direction can be used, such as a comb-like item.
Bras can also be angled towards the center or wavy to better hold hair.
The optical component window 310 may be perpendicular to the hair scan direction, thereby allowing averaging of readings from multiple hair fibers.
Source Calibration:
To obtain an exact spectrum of the hair, the lighting spectrum can be calibrated. The actual spectral measurement is that which is detected by the detector divided by the calibrated data at each wavelength after various offset signal subtraction corrections and non-linear correction have been applied.
However, the spectrum of the illuminated data need not be fixed. Temperature changes, small mechanical movement, LED intensity changes over time, and other reasons can affect the output spectrum.
The optical reader can thus support online calibration of the spectroscopy detector.
Referring now to Figure 39A, while part of the detector obtains illumination from the hair, part of the detector obtains a signal from the illumination module next to the grating without being reflected from the hair. The signal directly from the lighting module and the grid can be used for online calibration. Such a signal can be reflected from the targets in situ.
Calibration can be obtained by taking a single row from the calibrated area, or by averaging some or all of the rows in the calibration area. Other known statistical methods such as median or average without scatter points can also be used.
Calibrated data can be averaged over time, that is, determination of sensor calibration by using calibration measurements at different times.
The calibration area can be constructed of a single sensor part or regions, as shown in Figure 39A, calibration area 1 and calibration area 2. More than two regions can also be defined.
Lighting can be sampled from anywhere in lighting mode between grid and hair. Sampling can be carried out by a weak divider, such as 95/5% where 5% is done to the calibration area.
Calibration can be done every specific time or even for every spectrum measurement.
Polarization:
Illumination and detection modules can use polarized light in order to increase the signal-to-noise ratio and in order to improve the detection of relative amounts of material in the hair, including melanin, eumelanin, pheomelanin, hair dyes, water , etc.
The light module can illuminate hair at one or more of the following polarizations:
* Polarization parallel to the hair axis.
* Polarization perpendicular to the hair axis.
* linear polarization at any angle to the hair axis.
* circular polarization * any elliptical polarization
The optical reader can allow the change of the polarization of the illumination module by means of mechanical / optical or electronic switching. The change can be determined automatically or manually. For example, you can
ES 2 823 977 T3 have different polarizations that give better results for specific hair colors.
The detection module can detect reflected light by filtering or by passing any of the polarizations defined for the lighting module.
The change of polarization can be carried out in the lighting module or in the sensor.
Referring now to Figure 39B one method of polarization is to illuminate the hair in a given polarization and pass the same polarization into the detection module.
Referring now to Figure 39C, another method is to illuminate the hair at a given polarization and run the orthogonal polarization through the detection module. Either in one case or another, the polarization can be controlled by any element that changes the polarization: polarizer, wave plates (including λ / 2 and λ / 4), rotating polarizer prisms and non-linear elements and others.
The polarizing element in the light module can be placed anywhere between the light source and the hair. The polarizing element can still be part of the light source itself (for example, when using a polarized source).
The polarizing element in the detection module can also be placed anywhere between the hair and the sensor. It may still be part of the sensor detector.
The polarizer can have the same or different polarizing effect at different wavelengths.
The polarization of the illumination and / or detection module can be changed while the hair is scanned. An example is obtaining spectroscopy using two orthogonal polarizations, which can be advantageous when estimating relative amounts of material in the hair.
Polarization can be determined for a single light source, all light sources, or any part of them.
If there is more than one detector, the polarization can be determined for a single detector, all detectors or any part of them.
External Light Suppression:
Another problem that can affect the measurement is getting an external light signal hitting the hair and reaching the spectroscopy detector.
Since the external light is not directed, unlike the light from the illumination source and regardless of whether it is directed or not, undesirable signals from the hair due to the external light can reach the detector.
One solution is to take one or more spectrum measurements without using the hair reader's light sources. The spectrum thus obtained can then be subtracted from the spectrum measured when using the internal illumination source.
External light suppression measurements can be made at the beginning of the hair scan, at the end or even during the scan, after any or all of the illumination pulses.
III. The solid formulation:
Solid formulations suitable for use in treating hair are disclosed herein. According to some embodiments of the present invention, the solid formulations are in the form of tablets comprising a super-disintegrating agent, which confers advantageous elements to the tablet. The solid formulations disclosed herein may further comprise color-imparting agents (such as dye precursors, dye couplers, and direct dyes) and may be used in combination with, or may further comprise, other hair treating agents, such as alkaline agents and oxidizing agents.
In some embodiments, the solid formulations disclosed herein provide a group of basic shades in the form of fast-disintegrating tablets. Thus, basic tones are formulated individually as tablets, forming the color palette available to the end user, which can be combined in a varied way to obtain almost infinite possibilities of colors and tones.
Solid formulations in tablet form are easily and accurately measurable (for example, by counting) and therefore a desired final color formula can be reproducibly prepared by mixing specific amounts of appropriate base shade tablets by appropriate means,
ES 2 823 977 T3 optionally supplemented with alkaline and / or oxidizing agents and / or other agents useful in hair coloring. In some embodiments, part or all of the other active agents used in the coloring processes (such as alkaline agents, bleaching agents, oxidizing agents, and thickening agents) are provided in the same form of fast-disintegrating tablets.
The type (s) of color-imparting agents consisting of the appropriate base and medium shades and / or active agents to be combined therewith depends on the type of treatment sought.
For example, for permanent coloring, where the color-imparting agents penetrate the fiber to its cortex, the basic shade tablets predominantly but not exclusively comprise appropriate dye precursors and couplers, if necessary. Appropriate media for permanent coloring generally comprise alkaline and oxidizing agents, which can be provided in separate media and / or in separate tablets and / or within at least part of the color-imparting tablets used.
For temporary coloring, where the color-imparting agents remain on the fiber surface, the basic shade tablet formulations comprise predominantly, but not exclusively, direct dyes, whereby other active agents, such as oxidizing agents and alkaline agents , are not commonly used.
Semi-permanent and demi-permanent coloring correspond to intermediate situations where the basic tones can comprise all types of agents that give color, part of which remains on the surface of the fiber, where the external part can penetrate to some extent the cuticle of fiber (semi-permanent) or even the fiber cortex (demi-permanent). For semi-permanent coloring, the media generally comprise, if any, low levels of alkaline and oxidizing agents, which can be provided in separate media and / or in separate tablets and / or within at least part of the color-imparting tablets used. .
For demi-permanent coloring, the media generally comprise an oxidizing agent in a lower amount than for permanent coloring and an alkaline agent other than ammonia, both can be provided as separate media and / or in separate tablets and / or inside at least part of used color-imparting tablets.
Certain direct dyes, when used in conjunction with oxidative coloring processes, have sufficient fade resistance to be used for non-permanent coloring in the absence of precursors or couplers and therefore such direct dyes can be used alone, or in admixture with other dyes. direct, in basic tone tablets as provided herein.
The term "basic shade" refers to a color-imparting agent or a combination of color-conferring agents that provide a primary coloring shade that can be combined with one or more different base shades or primary shades to form a desired final color. Basic shades can be considered as the elemental coloring constituents of a palette. The term "basic shade" is also used herein to refer to a set of tablets characterized by a particular color-imparting agent or a combination of color-imparting agents.
According to one aspect of some embodiments of the invention, a solid formulation suitable for use in preparing a hair treatment composition is provided, the formulation is in the form of a tablet and comprises at least one super-disintegrating agent and at least one active agent selected from the group consisting of a color imparting agent, an alkaline agent, an oxidizing agent, and a thickening agent.
In some embodiments, a hair treating composition is a coloring composition, suitable for use (or useful) in coloring hair. Such compositions include both compositions comprising a color-imparting agent, as defined herein, and compositions that can be used in combination with a color-imparting agent, such as, but not limited to, compositions comprising any of the other agents. assets as described in this document. For example, compositions comprising an alkaline agent, which can facilitate the introduction of a color-imparting agent to hair, compositions comprising an oxidizing agent, which can react with dye intermediates to produce a dye, and compositions comprising a thickening agent , which provide a consistency that facilitates coloring by a color-imparting agent, are considered herein as hair treatment compositions.
In some of these embodiments, the active agent comprises a color-imparting agent.
The terms color-imparting agents, color-imparting compounds, color-imparting ingredients, and coloring agents are used interchangeably herein and encompass any compound used to impart a color by introducing a colored substance (eg, dye, pigment), including, but not limited to, oxidation dye precursors, oxidation dye couplers, direct dyes, and any combination thereof.
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Solid formulations comprising color-imparting agents can form basic tone tablets, as described herein.
In some embodiments, the solid formulation comprises, optionally in addition to the color-imparting agent, any of the other active agents mentioned above. Each of these active agents may be suitable for inclusion in a coloring composition when combined with a color-imparting agent either within the same solid formulation, in a different solid formulation, or in any other separate form (e.g., medium liquid such as an aqueous solution).
In some embodiments, at least one color-imparting agent is present as an active agent in a solid formulation as described herein, for example, in order to form a color imparted by a coloring composition.
In some embodiments, at least one alkaline agent is present as an active agent in a solid formulation, as described herein, for example, in order to cause the hair to swell, thereby facilitating penetration of the conferring agent. color to the fibers.
In some embodiments, at least one oxidizing agent is present as an active agent in a solid formulation as described herein, for example, in order to oxidize the dye precursors in a coloring composition and / or in order to bleaching a color in the hair (for example, natural pigmentation).
In some embodiments, at least one thickening agent is present as an active agent in a solid formulation as described herein, for example, in order to obtain a consistency of the coloring composition that is highly suitable to be applied to and remain in contact with a surface to be colored (eg relatively high viscosity) with little or no sag, dripping, etc.
In some embodiments, a solid formulations tablet form is formed from a powder and / or granules, for example, by compressing the powder and / or granules. Tablet forms can have various porosities and cohesiveness that ultimately impact their disintegration rate (eg, on contact with a liquid).
The solid formulation in tablet form is also referred to herein interchangeably as tablet formulation, solid formulation, and simply as tablet.
In some embodiments, the maximum width of a tablet is in a range of 2mm to 10mm. In some embodiments, the maximum width of the tablet is in a range of 3mm to 7mm. In some embodiments, the maximum width of the tablet is in a range of 4mm to 6mm.
In some embodiments, the maximum width and minimum width of a tablet are each in a range of 2mm to 10mm. In some embodiments, the maximum width and the minimum width of a tablet are each in a range of 3mm to 7mm. In some embodiments, the maximum width and the minimum width of a tablet are each in a range of 4mm to 6mm.
In some embodiments, the average diameter of the tablet is in a range of 2mm to 10mm. In some embodiments, the average diameter of the tablet is in a range of 3mm to 7mm. In some embodiments, the average diameter of the tablet is in a range of 4mm to 6mm. Average diameters are calculated based on diameters that pass through the geometric center of the tablet.
Each of the tablet formulations disclosed herein can be of any geometric shape, as long as the tablets can be individually measured. Suitable shapes include, for example, spheres, cylinders, cubes, discs, and ellipses and similar spheroid, cuboid, discoid, and ellipsoid shapes. Spheroid, cylindrical, and discoid shapes can have oval or circular cross-section. The shapes can be flattened or elongated, which in the case of a spheroid having a circular cross section would mean that the thickness of the tablet is respectively more or less the diameter of the tablet. The tablets may also be marked with an indented or embossed emblem, brand or other type of marking or identification.
The extent of flattening or elongation of the tablet shape must be compatible with the contemplated delivery of the tablets. In some embodiments, tablets for automatic delivery are slightly flattened or elongated, maintaining an approximate symmetrical shape.
In some embodiments, the tablets have convex or rounded outer surfaces. Such tablets are expected to flow or roll over one another more easily than tablets with flat or concave outer surfaces. Tablets that easily flow or roll over one another can facilitate delivery (eg, with a device described herein).
ES 2 823 977 T3
In some embodiments, a solid formulation is substantially spherical or spheroidal, characterized by an average diameter as described herein.
Various compounds (generally referred to as disintegrants) can be included in a tablet in order to increase the rate of disintegration.
In accordance with some embodiments of the present invention, the tablet formulations disclosed herein comprise a super-disintegrating agent. Such formulations are uniquely characterized as fast disintegrating tablets. Herein and in the art, a superdisintegrant refers to a class of disintegrant that is particularly effective in inducing disintegration of a solid formulation (eg, a tablet). In contrast to many disintegrants, superdisintegrants are commonly effective at low concentrations. Of course, in contrast to most other types of disintegrant, high concentrations of superdisintegrant can lead to slower disintegration of the solid formulation.
Thus, in some embodiments, the concentration of the superdisintegrant in a solid formulation described herein is less than 10 percent by weight, for example, in a range of 0.5 to 10 percent by weight. In some embodiments, the concentration of the super-disintegrating agent in a solid formulation described herein is less than 5 percent by weight, for example, in a range of 0.5 to 5 percent by weight. In some embodiments, the concentration of the super-disintegrating agent in a solid formulation described herein is less than 3 percent by weight, for example, in a range of 0.5 to 3 percent by weight.
The use of such low concentrations is advantageous because, for example, an agent that provides advantageously rapid disintegration of the solid formulation is less likely, being at a low concentration, to interfere with the function of other ingredients in a coloring composition. . Such interference can be, for example, interaction with other agents in the formulation, which can lead to the formation of toxic or dangerous compounds and / or promote such interactions and / or interfere with interactions between other agents in the formulation (for example, dye couplers and dye precursors).
Superdisintegrating agents are known as hygroscopic compounds that act by absorbing liquid (eg, water) from a medium when brought into contact with the medium (eg, an aqueous medium). Such absorption induces disintegration by causing considerable swelling of the super-disintegrating agent and / or by enhancing capillary action. A swelling pressure exerted by superdisintegrating agents swollen in an external or radial direction can cause a tablet to burst.
Suitable superdisintegrating agents in accordance with some embodiments of the present invention include, but are not limited to, superdisintegrating agents that are characterized by a water absorption ratio of at least 0.5. The water absorption ratio is defined as the change in weight following wetting of the tablet divided by the weight of the dry tablet.
In some embodiments, the super-disintegrating agent is characterized by a water absorption ratio of at least 0.6, at least 0.7, at least 0.8, and at least 0.9. Superdisintegrating agents suitable for use in embodiments of the present invention can also be characterized by a water absorption ratio of 1.0, 1.2., 1.2, 1.3, 1.4, 1.5 and even by a higher water absorption ratio of, for example, 2.0.
In some embodiments, the superdisintegrating agent is characterized by a water absorption ratio ranging from about 0.5 to about 2. In some embodiments, the superdisintegrating agent is characterized by a water absorption ratio ranging from about 0.5 to about 1.5. In some embodiments, the super-disintegrating agent is characterized by a water absorption ratio ranging from about 0.6 to 0.9. Any intermediate value within these ranges is contemplated.
However, the aforementioned hygroscopy of super-disintegrating agents renders such super-disintegrating agents incompatible for use with moisture-sensitive ingredients, particularly in formulations that are designed to have a long shelf life.
The present inventors have surprisingly discovered that superdisintegrating agents that are a priori incompatible with color-imparting agents (which are generally sensitive to moisture) are suitable for inclusion in solid formulations according to embodiments of the invention. Despite the hygroscopicity of the super-disintegrating agent, the solid formulations described herein were shown to exhibit an appropriately long shelf life, while exhibiting a desirable disintegration rate of a few seconds (when uncoated).
The super-disintegrating agent according to some embodiments of the invention is substantially insoluble in water, such that the super-disintegrating agent remains intact after contact with an aqueous medium (also as many media comprising hydrophilic solvents). By remaining intact, the superdisintegrating agent maintains its ability to induce disintegration.
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Herein, insoluble in water refers to a solubility of less than 10 grams per kg of water (at 25 ° C and pH 7). Thus, in some embodiments, a compound that is insoluble in water, under the indicated condition, at a concentration of more than 10 grams per Kg of water is considered insoluble in water.
In some embodiments, the solubility of a superdisintegrant is less than 3 grams per kg of water (at 25 ° C and pH 7). In some embodiments, the solubility of a super-disintegrating agent is less than 1 gram per kg of water (at 25 ° C and pH 7). In some embodiments, the solubility of the super-disintegrating agent is less than 0.3 grams per kg of water (at 25 ° C and pH 7). In some embodiments, the solubility of the super-disintegrating agent is less than 0.1 grams per kg of water (at 25 ° C and pH 7).
Examples of such water-insoluble superdisintegrating agents include a variety of cross-linked polymers. In some embodiments, a polymer that is fairly hydrophilic (eg, an ionic polymer) interacts abundantly with water molecules, but does not dissolve in water due to steric hindrance caused by crosslinking.
It will be appreciated that such water-insoluble superdisintegrating agents may be chemically similar to polymers used for other purposes, except with respect to solubility in water. For example, many water-soluble hydrophilic polymers are used as thickening agents, since dissolution of such a polymer allows a polymer to fully spread into a liquid medium to be thickened.
Suitable superdisintegrating agents include, without limitation, cross-linked celluloses such as croscarmellose (Cross-linked carboxymethyl cellulose, which is commonly used as a sodium salt), for example, Ac-Di-Sol®, Explocel®, Nymcel ZSX®, Pharmacel® XL, Primellose ®, Solutab® and Vivasol® super disintegrating agents; crospovidone (cross-linked polyvinylpyrrolidone), eg, crospovidone M®, Kollidon® and Polyplasdone® super disintegrating agents; cross-linked starch, such as sodium starch glycolate, for example, Explotab®, Explotab® CLV, Explosol®, Primojel®, Tablo® and Vivastar® super disintegrating agents; cross-linked alginic acids, eg, Satialgine® super disintegrating agent; cross-linked polyacrylic compounds such as ion exchange resins, eg, Indion® 414, Tulsion® 339 and Amberlite® IRP resins; and some polysaccharides, such as soybean polysaccharide, for example Emcosoy® superdisintegrating agent.
Exemplary superdisintegrating agents include croscarmellose sodium (eg, Ac-Di-Sol®), crospovidone (eg, Polyplasdone®), and sodium starch glycolate (eg, Primojel®).
Calcium silicate is an example of a non-polymeric super-disintegrating agent. Calcium silicate is a relatively inert mineral characterized by high water absorption and can be included in some embodiments of the solid formulation at a concentration of up to 40 percent by weight, for example, in a range of 20 to 40 percent. in weigh. However, it is generally less effective than crosslinked polymeric superdisintegrating agents at low concentrations.
In addition to super-disintegrating agents, additional materials included in some embodiments of the solid formulation described herein (eg, excipients) may contribute to the disintegration properties of the solid formulation, although this may not be the primary function of the additional material. . Such materials are referred to herein as disintegration aids.
In some embodiments, an auxiliary disintegration agent is soluble in water. In some such embodiments, rapid dissolution of the disintegration aid in an aqueous medium (as well as many media comprising hydrophilic solvents) facilitates disintegration of the solid formulation.
In some embodiments, an auxiliary disintegration agent is characterized by low compressibility and cohesiveness, which improves the porosity of the tablet and thus facilitates disintegration of the tablet via capillary action. For example, capillary action can allow a surrounding aqueous medium to penetrate a tablet through your pores. The infiltration medium fills the pores, dissolving the water soluble ingredients (including, in some embodiments, the disintegrating aid itself), weakening the interparticle or intergranular physical bonds, and / or swelling the super-disintegrating agent.
Water soluble disintegration aids associated with high tablet porosity can be obtained, for example, by spray drying or agglomeration of water soluble agents. Examples of such disintegration aids include spray-dried lactose monohydrate (eg, SuperTab® 11SD and SuperTab® 14SD excipients), spray-dried mannitol (eg, Mannogem® excipient), and agglomerated isomalt (eg, galenlQ® 720 excipients). and galenlQ® 721).
aluminum magnesium silicate is an exemplary disintegration aid.
In some embodiments, the concentration of aluminum magnesium silicate in a tablet when uncoated
ES 2 823 977 T3 is in a range of 5 to 40 percent by weight. In exemplary embodiments, the concentration of the aluminum magnesium silicate in a tablet when uncoated is in a range of 10 to 22 percent by weight.
In some embodiments, a disintegration aid is a binder that exhibits an intrinsic disintegration property. Examples of such binders include starch and cellulose.
Other types of disintegration aids that may be included in some embodiments of the invention include exothermic agents (air expansion), non-swelling agents (electrical repulsive force), gas release agents, and enzyme systems.
In some embodiments, the concentration of the disintegration aid is at least 10 percent by weight, or at least 15 percent by weight of the tablet (when uncoated). Higher concentrations of such an agent usually correlate with faster disintegration.
In some embodiments, the active agent (s) comprise at least one color-imparting agent. In some embodiments, the color confer is selected to be appropriate for coloring the hair. In some embodiments, a color-imparting agent is selected to be appropriate for coloring human hair (eg, appropriately non-toxic when applied to the head of a human).
It will be appreciated that fast disintegration tablets are particularly advantageous for tablets comprising color imparting agents. For example, rapid disintegration facilitates the mixing of different color-imparting agents (eg, in different types of tablets) in a homogeneous manner, as it is important in the preparation of a coloring composition. Furthermore, the rapid disintegration ensures that the oxidation of all oxidation dye intermediates begins concurrently, thus avoiding the formation of undesirable by-products, or of dyes that will not penetrate the hair shaft due to the increased molecular size. As noted hereinabove, obtaining fast disintegrating tablet formulations containing color-imparting agents is not a trivial task.
Examples of appropriate types of color-imparting agents that can be included in a solid formulation as described herein include a direct dye, a dye precursor, and a dye coupler. Such agents can be included in a solid formulation in any combination thereof, as discussed in more detail herein.
In some embodiments, a dye precursor is included in combination with a dye coupler, such that a solid formulation comprises at least one direct dye, and / or a combination of at least one dye precursor and at least one dye coupler. dye.
Oxidation dye intermediates, either dye precursors or dye couplers, are generally aromatic ring or heteroaromatic ring derivatives, being mostly aromatic diamines, aminophenols, phenols and / or naphthols.
Oxidation dye intermediates that are capable of deep-toning white hair are commonly classified as dye precursors. Such precursors generally have two amine groups, and / or an amine group and a hydroxy group, at mutually selected positions. Dye precursors are generally aromatic diamines, diaminophenols and / or aminophenols with an amine or hydroxy group ortho or para to an amine group. Derivatives of pyrimidine and pyrazole (eg, substituted pyrimidine, substituted pyrazole), used to develop shades with red highlights, are also generally considered as dye precursors.
Herein, an aromatic diamine refers to a compound comprising an aromatic ring substituted by at least two amine groups.
As used herein, the terms diaminophenols and a diaminophenol encompass any compound that is a substituted phenol, wherein at least two phenol ring Substituents are amine groups.
As used herein, the terms aminophenols and an aminophenol encompass, any compound that is a substituted phenol, wherein at least one phenol ring substituent is an amine group.
Dye couplers are oxidation dye intermediates that, by themselves, produce only weak coloring through oxidation, but can be combined with dye precursors to produce stronger shades. The amine and / or hydroxy groups that substitute dye couplers are frequently meta to each other. Dye couplers include m-phenylene diamines, m-aminophenols, naphthols, resorcinols, polyphenols, pyrazolones, and their derivatives.
As used herein, the terms m-phenylene diamines and an m-phenylene diamine encompass substituted and unsubstituted m-phenylene diamine.
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As used herein, the terms m-aminophenols and an m-aminophenol encompass substituted and unsubstituted m-aminophenol.
As used herein, the terms naphthols and a naphthol encompass substituted and unsubstituted 1-naphthol and 2-naphthol.
As used herein, the terms resorcinols and a resorcinol encompass resorcinol (substituted and unsubstituted benzene-1,3-diol).
As used herein, the term polyphenol encompasses compounds combined to a large extent of covalently linked phenol groups (that is, aromatic rings substituted by at least one hydroxyl group). In some embodiments, a polyphenol is characterized as having at least 5 aromatic rings and at least 12 hydroxyl groups connected to aromatic rings, per 1,000 Da molecular weight. In some embodiments, the molecular weight of a polyphenol is at least 500 Da.
A wide variety of dye precursors and dye couplers, suitable for use in preparing a coloring composition, will be known to the skilled person.
When dye precursors and dye couplers are used in combination (for example, as active agents in a solid formulation), the dye couplers must be compatible with the dye precursors that are used, that is, they can react chemically to form a coloring agent.
Examples of suitable oxidation dye precursors, which can be used alone or in admixture with one another, include, without limitation, 1,3-bis [(4-aminophenyl) (2-hydroxyethyl) amino] -2-propanol; 1,4-bis [(4-aminophenyl) amino] butane; 1,4-diamino2- (1-methylethyl) benzene; 1,4-diamino-2- (2-hydroxyethoxy) benzene; 1,4-diamino-2- (2-hydroxyethyl) benzene; 1,4-diamino-2 (pyridin-3-yl) benzene; 1,4-diamino-2- (thiophen-2-yl) benzene; 1,4-diamino-2- (thiophen-3-yl) benzene, U, 4-diamino-2,3-dimethylbenzene; 1,4-diamino-2,5-dimethylbenzene; 1,4-diamino-2,6-dimethylbenzene; 1,4-diamino-2-aminomethylbenzene; 1,4-diamino-2-hydroxymethyl-benzene, -1,4-diamino-2-methoxymethyl-benzene; 1,4-diamino-3,5-diethylbenzene; 1,8-bis (2,5-diaminophenoxy) -3,6-dioxa-octane; 1 - [(4-chlorophenyl) methyl] -4,5-diamino-1H-pyrazole; 1-hydroxyethyl-4,5-diaminopyrazole; 2- (2-Cacetylamino) ethoxy) -1,4-diamino-benzene; 2-propylamino-5-aminopyridine; 2,4,5,6-tetraminopyrimidine; 2,5,6-triamino-4- (IH) -pyrimidone; 2,5-diamino-biphenyl; 2,5-diaminopyridine; 2-amino-5-ethoxyphenol; 2-amino5-methylphenol; 2-amino-6-methylphenol; 2-aminophenol; 2-chloro-1,4-diamino-benzene; 2-chloro-p-phenylenediamine; 2-p-hydroxyethyl-p-phenylenediamine; 4,5-diamino-1- (1-methylethyl) -1H-pyrazole; 4,5-diamino-1- (2-hydroxyethyl) -1H-pyrazole; 4,5-diamino-1 - [(4-methylphenyl) methyl] -1H-pyrazole; 4,5-diamino-1-methyl-1H-pyrazole; 4 - [(2,3-dihydroxypropyl) amino] aniline; 4 - [(2-methoxyethyl) amino] aniline; 4 - [(3-hydroxypropyl) amino] aniline; 4- [di (2-hydroxyethyl) amino] -2-methylaniline; 4- [di (2-hydroxyethyl) amino] aniline; 4- [ethyl (2-hydroxyethyl) amino] aniline; 4-amino-2- (2-hydroxyethyl) phenol; 4-amino-2- (aminomethyl) phenol; 4-amino-2- (hydroxymethyl) phenol; 4-amino-2- (methoxymethyl) phenol; 4-amino-2 - [(2-hydroxyethyl) amino] methylphenol; 4-amino-2-fluorophenol; 4-amino-2-methylphenol; 4-amino-3- (hydroxymethyl) phenol; 4-amino-3-fluorophenol; 4-amino-m-cresol; 4-diethylaminoaniline; 4-dimethyIaminoaniline; 4-dipropylaminoaniline; 4-methyl-aminophenol; 4-phenylaminoaniline; 5-aminosalicylic acid; 6-amino-m-cresol; hydroxyethyl-p-phenylenediamine; hydroxypropyl-bis (hydroxyethyl) -p-phenylenediamine; N, Nbis (2-hydroxyethyl) -p-phenylenediamine; N-phenyl-p-phenylenediamine; o-aminophenol; p-aminophenol; p-methylaminophenol; pphenylenediamine; toluene-2,5-diamine; and you get out of them.
Exemplary dye precursors include 4-amino-m-cresol, p-aminophenol, N, N-bis (2-hydroxyethyl) -p-phenylenediamine (e.g., as a sulfate salt), 1-hydroxyethyl-4,5- diaminopyrazole (eg, as a sulfate salt) and toluene2,5-diamine (eg, as a sulfate salt).
Examples of suitable dye couplers, which can be used alone or in admixture with one another, include, without limitation, 1- (2-aminoethoxy) -2,4-diaminobenzene; 1,2,4-trihydroxy-5-methyl-benzene; 1,2,4-trihydroxybenzene; 1,2-dichloro-3,5-dihydroxy-4-methiIbenzene; 1,3-di (2,4-diaminophenoxy) propane; 1,3-diamino-2,4-dimethoxybenzene; 1,3-diamino-4- (2,3-dihydroxy-propoxy) benzene; 1,3-diaminobenzene, -1,3-dihydroxy-2-methylbenzene; 1,3-dihydroxy-benzene; 1,5-dichloro2,4-dihydroxybenzene; 1,5-dihydroxy-naphthalene; 1,5-naphthalene diol; 1,7-dihydroxynaphthalene; l-acetoxy-2-methylnaphthalene, -1-chloro-2,4-dihydroxybenzene; 1-naphthol; 2- (4-amino-2-hydroxyphenoxy) ethanol; 2,3-diamino-6-methoxypyridine, · 2,3-dihydroxynaphthalene; 2,3-indoleindione; 2,4-di [(2-hydroxyethyl) amino] -1,5-dimethoxybenzene; 2,4-diamino-1- (2-hydroxyethoxy) 5-Inethylbenzene; 2,4-diamino-1- (2-hydroxyethoxy) benzene; 2,4-diamino-1,5-di (2-hydroxyethoxy) benzene; 2,4-diamino-1ethoxy-5-methylbenzene; 2,4-diamino-1-fluoro-5-methylbenzene; 2,4-diamino-1-methoxy-5-methylbenzene; 2,4-diaminophenoxyacetic acid; 2,4-diaminophenoxyethanol; 2,6-bis (2-hydroxyethyl) aminotoluene; 2,6-diamino-3,5-dimethoxypyridine; 2,6-diaminopyridine; 2,6-dihydroxyethyIaminotoluene; 2,6-dimethoxy-3,5-pyridinediamine; 2,7-dihydroxy-naphthalene; 2 - [(3-hydroxyphenyl) amino] acetamide; 2-amino-1- (2-hydroxyethoxy) -4-methyIaminobenzene; 2-amino-3-hydroxypyridine; 2-amino-3-hydroxypyridine; 2-amino-4 - [(2-hydroxyethyl) amino] anisole; 2-amino-4-hydroxyethylamino-anisole; 2-chloro-1,3-dihydroxybenzene; 2-methyl-1-naphthol; 2-methyl-1-naphthol acetate; 2-methyl-1-naphthol; 2-methyl-5-hydroxyethylaminophenol; 2-methylresorcinol; 3,4-diaminobenzoic acid; 3,4-dihydro-6-hydroxy-1,4 (2H) -benzoxazine; 3,4-methylenedioxy-aniline; 3,4 methylene dioxyphenol; 3,5-diamino-2,6-dimethoxy-pyridine; 3 - [(2,3-dihydroxy-propyl) amino] -2-methylphenol; 3 - [(2-aminoethyl) amino] aniline; 3 - [(2-hydroxyethyl) amino] -2-methylphenol; 3 - [(2-hydroxyethyl) amino] aniline; 3 - [(2-hydroxyethyl) amino] phenol; 3 - [(2-methoxyethyl) amino] phenol; 3- [di (2-hydroxyethyl) amino] aniline; 3-amino-2,4-dichlorophenol; 3-amino-2-chloro-6
ES 2 823 977 T3 methylphenol; 3-amino-2-methylphenol; 3-amino-6-methoxy-2- (methylamino) pyridine; 3-aminophenol; 3-diethylaminophenol; 3dimethylaminophenol; 3-methyl-1-phenyl-5-pyrazolone; 4- (2-hydroxyethyl-amino) -2-methylphenol; 4-amino-2-di [(2-hydroxyethyl) amino] 1-ethoxybenzene; 4-amino-2-hydroxytoluene; 4-Chlororesorcinol; 4-hydroxyindole; 5,6-dihydroxyindole; 5,6-dihydroxyindoline; 5 - [(2-hydroxyethyl) amino] -1,3-benzodioxole; 5 - [(2-hydroxyethyl) amino] -2-methylphenol; 5 - [(2-hydroxyethyl) amino] 4-methoxy-2-methylphenol; 5 - [(3-hydroxypropyl) amino] -2-methylphenol; 5-amino-2,4-dichlorophenol; 5-amino-2-ethylphenol; 5-amino-2-methoxyphenol; 5-amino-2-methylphenol; 5-amino-4-chloro-2-methylphenol; 5-amino-4-ethoxy-2-methylphenol; 5-amino-4-fluoro-2-methylphenol; 5-amino-4-methoxy-2-methylphenol; 5-amino-6-chloro-o-cresol; 5-hydroxyindole; 5-methyl-2- (1-methylethyl) phenol; 5-methyl2-aminophenol; 6-amino-3,4-dihydrol, 4 (2H) -benzoxazine; 6-bromo-1-hydroxy-3,4-methylenedioxybenzene; 6-hydroxyindole; 7-hydroxyindole; di (2,4-diaminophenoxy) methane; hydroquinone; hydroxy-benzomorpholine; Hydroxyethyl-3,4-Tenethylenedioxyaniline; m-aminophenol; m-phenylene diamine; N- (3-dimethylaminophenyl) urea; resorcinol; and you get out of them.
Exemplary dye couplers include 4-amino-2-hydroxytoluene, m-aminophenol, 2,4-diaminophenoxyethanol (for example, as a dihydrochloride salt), resorcinol, and hydroxyethyl-3,4-methylenedioxyaniline (for example, as a salt of hydrochloride).
It will be noted that certain color-imparting agents can be considered in the art as either dye precursors or dye couplers. This is the case in particular for some self-coupling dye intermediates (for example, 2-amino-3-hydroxypyridine, 2-amino-6-methylphenol, 2-amino-5-ethoxyphenol, 2-propylamino-5-aminopyridine and 5 -methyl-2-aminophenol).
In some embodiments, the dye precursor (or mixture of dye precursors) and the dye coupler (or mixture of dye couplers) are used in approximately equimolar amounts, that is, a ratio of the molar concentration of dye precursor (either a dye precursor or a sum of the concentration of a plurality of dye precursors) and the molar concentration of the dye coupler (either a dye coupler or the sum of the concentration of a plurality of dye couplers) are approximately 1: 1 (eg, 2: 3 to 3: 2, 4: 5 to 5: 4).
However, depending on the availability of appropriate binding sites, non-equimolar properties may also be appropriate. For example, blocked couplers can bind to only one precursor, while unblocked couplers, such as resorcinol, can bind to two precursor molecules.
Thus, in some embodiments, the molar ratio of the dye precursor and dye coupler is in a range of 2: 1 to 1: 2.
As is known to those skilled in the art of hair coloring, certain dye precursors can have a toxicological effect that is uncoupled. Here, in some embodiments, such dye precursor is combined with a slight molar excess, eg, up to 2% excess, of at least one appropriate dye coupler.
In some embodiments, an oxidation dye intermediate (ie, a dye precursor or dye coupler) is used alone, for example when the intermediate is self-coupling. In some embodiments, the dye precursor is used as a color imparting agent without a dye coupler.
Combinations of dye precursors and dye couplers to form larger colored molecules (oxidation dyes) can comprise two or more dye intermediates. For example, pairs and trios of dye intermediates (e.g. dimers or trimers are formed) may comprise one type of precursor for one type of coupler, one type of precursor for two types of couplers, and two types of couplers for one type of coupler. coupler.
Appropriate pairs or trios of precursors and couplers are known in the coloring art and depend on the chemical structure of each component. For example, the precursors selected from the group consisting of:
1-hydroxyethyl-4,5-diamino pyrazole, 2-chloro-p-phenylenediamine, 2-p-hydroxyethyl-p-phenylenediamine, 4-amino-m-cresol, hydroxypropyl-bis (hydroxyethyl) -p-phenylene-diamine; N, N-bis (2-hydroxyethyl) -p-phenylenediamine; N-phenyl-p-phenylenediamine, oaminphenol, p-aminophenol, p-methylaminophenol, p-phenylenediamine; toluene-2,5-diamine and salts thereof, each can be coupled with any coupler selected from the group consisting of:
1,5-naphthalene diol, l-naphthol; 2,4-diaminophenoxyethanol: 2,6-diaminopyridine; 2,6-dimethoxy-3,5-pyridinediamine; 2-amino-3-hydroxypyridine; 2-amino-4-hydroxy-ethylamino-anisole; 2-methyl-1-naphthol; 2-methyl-5-hydroxyethylaminophenol; 2-methylresorcinol, 3-aminophenol; 4- (2-hydroxyethyl-amino) -2-methylphenol; 4-amino-2-hydroxytoluene; 5-amino-6-chloro-ocresol; 5-methyl-2-aminophenol; 6-hydroxyindole; hydroquinone; hydroxybenzomorpholine; hydroxyethyl-3,4-methylenedioxyaniline, m-aminophenol, resorcinol, and salts thereof.
Exemplary precursor-coupler combinations include:
Toluene-2,5-diamine (eg, as a sulfate), m-aminophenol, and resorcinol; 1-hydroxyethyl-4,5-diaminopyrazol (for example, as a sulfate) and 4-amino-2-hydroxytoluene, N, N-bis (2-hydroxyethyl) -p-phenylenediamine (for example, as a sulfate) and 4 -amino-2-hydroxy-toluene;
ES 2 823 977 T3
N, N-bis (2-hydroxyethyl) -p-phenylenediamine (for example, as a sulfate) and 2,4-diamino-phenoxy-ethanol (for example, as a dihydrochloride);
4-amino-m-cresol and 4-amino-2-hydroxytoluene;
p-aminophenol and 4-amino-2-hydroxy-toluene;
toluene-2,5-diamine (for example, as a sulfate), 2,4-diaminophenoxyethanol (for example, as a dihydrochloride) and hydroxy-3,4-methylenedioxyaniline (for example, as a hydrochloride) and toluene-2,5- diamine (eg, as sulfate) and hydroxy-3,4-methylene-dioxyaniline (eg, as hydrochloride.
In some embodiments, a color-imparting agent in a solid formulation comprises at least one dye precursor and at least one dye coupler (eg, as described herein).
In some embodiments, the dye precursors and / or dye couplers are divided between different solid tablet-type formulations that can be used in combination with each other to form a coloring composition, for example in an appropriate molar ratio (e.g., a described ratio in the present document). An appropriate molar ratio can be obtained by selecting an appropriate number of each type of tablet.
Direct dyes according to embodiments of the invention can be natural direct dyes (eg henna) and / or synthetic direct dyes (eg nitro-, azo-, azine- and anthraquinone type dyes). At least one direct dye may be included in a solid formulation described herein as the sole color-imparting agent or in addition to oxidative dye intermediates (eg, dye precursors and / dye couplers) as described herein. document.
In some embodiments, at least one appropriate direct dyeing agent is included in a solid formulation comprising oxidation dye intermediates in order to advantageously modify hue, brilliance, color intensity, or coloration stability obtained from the use of dye intermediates. oxidation.
It will be appreciated that direct dyes to be used in combination with oxidizing agents (eg, agents used to oxidize oxidation dye intermediates) must be selected to be sufficiently resistant to oxidation.
In some embodiments, direct dyes are the only color-imparting agent in the solid formulation. In some embodiments, such a solid formulation is suitable for preparing a temporary coloring composition. In some embodiments, such a solid formulation is suitable for preparing a longer lasting coloring composition (eg, semi-permanent coloring and / or demi-permanent composition).
Examples of suitable natural direct dyes that can be used alone or in admixture with other dyes (eg, direct dyes), include without limitation alizarin, alkan, alkanine, anthocyanin, apigenin, apocarotenal, atromenthin, awobamine, berberine, betanine, bixin, extract black tea, Brazilian wood, butine / butein, chamomile, canthaxanthin, capsanthin, carajuirin, carotene, catechin, chlorophyll A / B, crocetin, curcumin, datiscetin, deoxysanthalin, drachorodine, emblica extract, tisetine, fukugetine, gossipetin, green tea extract, hemantine, indigo, isoramnetin, juglone, kaempferol, Iapacol, Iawsona, wood trunk extract, Iuteolin, Iicopene, wood, malclurin, morina, morindadiol, morindanigrina, munjistina , Naphthalene, Orcein, Purpuroxanthin, Quercetin, Redwood Sandalwood, Rhamnazine, Rhamnetin, Rhamnocitrine, Riboflavin, Rotlerin, Rubiadin, Rubietic Acid, Rutin, White Tea Extract, Xanthones, Xanthophyll and Zantoramnine.
Appropriate synthetic direct dyes that can be used alone or in mixtures with other dyes (for example, direct dyes) include without limitation anionic dyes, cationic dyes, nitro aromatic dyes, azine dyes (including indulins and nigrosines), azo dyes, triphenylmethane dyes and quinone dyes.
Examples of suitable synthetic dyes include, without limitation, 2-amino-6-chloro-4-nitrophenol; 2-hydroxyethyl picramic acid; 2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine, · 3-nitro-p-hydroxyethylaminophenol; 4-amino-3-nitrophenol; 4-hydroxypropylamino-3-nitrophenol; 4-nitro-o-phenylenediamine; hydroxyethyl-2-nitro-p-toluidine; N, N'-bis (2-hydroxyethyl) -2-nitro-pphenylene diamine; acid black 1; acid blue 1; acid blue 3; acid blue 62; acid blue 74; acid blue 74, aluminum lake; acid blue 9; acid blue 9 aluminum lake; acid blue 9 ammonium salt; acid green 1; green acid 25; acid green 50; acid orange 6; acid orange 7; acid red 14; acid red 14 aluminum lake; acid red 18; acid red 18 aluminum lake; acid red 184; acid red 27; Acid Red 27 Aluminum Lacquer; acid red 33; acid red 51; acid red 52; acid red 87; acid red 92; acid red 95; acid violet 43; acid violet 9; acid yellow 1; acid yellow 23; Acid Yellow 23 Aluminum Lake; acid yellow 3; Acid Yellow 3 Aluminum Lake; acid yellow 73; acid yellow 73 sodium salt; basic blue 26; basic blue 99; basic coffee 16; basic coffee 17; basic orange 31; basic orange 69, basic red 1; basic red 1: 1; basic red 51; basic red 76, - basic violet 11: 1, - basic violet 14; basic violet 16; basic violet 2; basic yellow 40; basic yellow 57, basic yellow 87; blue lacquer 1; glossy black 1; chromium hydroxide green; chromium oxide green; red curry; direct blue 86; disperse black 9; disperse blue 377; disperse red 17; disperse violet 1; disperse violet 15; Solid green FCP; Ferric Ammonium Citrate; HC Blue # 11; HC Blue # 12; HC Blue # 13; HC Blue # 14; HC Blue # 15; HC Blue # 16; HC Blue # 2; HC Blue # 7; HC Orange # 1; HC Orange # 2; HC Orange # 5; HC Red # 1; HC Red # 10; HC Red # 11; HC Red # 13; Red
ES 2 823 977 T3
HC # 14; HC Red # 15; HC Red # 3; HC Red # 7; HC Violet # 1; HC Violet # 2; HC Yellow # 10; HC Yellow # 13; HC Yellow # 14; HC Yellow # 15; HC Yellow # 2; Yellow HC # 4; HC Yellow # 7; Yellow HC # 9; pigment blue 15; Pigment Green 7; pigment red 4; pigment red 5; pigment red 48; pigment red 57; pigment red 57: 1; pigment red 63: 1; pigment red 64: 1; pigment red 88; red pigment 90: 1 aluminum lake; pigment red 112; pigment red 190; violet pigment 19; pigment violet 23; yellow pigment 13; solvent green 3; solvent green 7; solvent orange 1; solvent red 23; solvent red 3; Solvent Red 43; Solvent Red 48; solvent red 72; solvent red 73; solvent violet 13; Solvent Yellow 172; solvent yellow 18; solvent yellow 29; Solvent Yellow 33; Solvent Yellow 85; sunset yellow; tetraaminopyrimidine sulfate; groceries; red tub 1 and salts thereof.
Exemplary direct dyes include 2-amino-6-chloro-4-nitrophenol, 2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine, HC Blue # 15, HC Red # 10, red HC n<sup>or</sup> 11 and HC Yellow # 13.
In some embodiments, the concentration of the color imparting agent in the solid formulation is in the range of 0.01 to 40 percent by weight of the tablet when uncoated. In some embodiments, the concentration is in a range of 0.5 to 25 percent by weight of the tablet when uncoated.
In some embodiments, the concentration of all dye precursors in the solid formulation is in a range of 0.01 to 25 percent by weight of the tablet when uncoated. In some embodiments, the concentration is in a range of 0.1 to 15 percent by weight of the tablets when uncoated. In some embodiments, the concentration is in the range of 0.1 to 5 percent by weight of the tablet when uncoated.
In some embodiments, the concentration of all dye precursors in the solid formulation is in a range of 0.01 to 15 percent by weight of the tablet when uncoated. In some embodiments, the concentration is in a range of 0.01 to 10 percent by weight of the tablet when uncoated.
In some embodiments, the molar ratio of dye precursor to dye coupler ranges from 0.1 to 10 or 0.5 to 5 or 0.5 to 1.5 or 0.5 to 1 or 0.9 to 1. A ratio of about 1 or less is desirable in order to avoid the possible formation of hazardous compounds.
In some embodiments, the concentration of the direct dye in the solid formulation is in the range of 0.01 to 15 percent by weight of the tablet when uncoated. In some embodiments, the concentration is in a range of 0.1 to 10 percent of the tablet when uncoated. Herein, the phrase "percent by weight of the tablet when uncoated" means that the formulation is in the form of a coated tablet, only the uncoated portion of the tablet is taken into account when calculating the percent by weight of the component ( eg, dye precursor). Thus, any color-imparting agents that are present in the coating are not taken into account.
In some embodiments, the active agent (s) in a solid formulation consist of a color-imparting agent (s) (eg, as described herein), that is, the Formulation does not include other types of active agents described herein.
In some embodiments, the active agent (s) in the solid formulation comprise at least one alkalizing agent.
In some embodiments, the alkaline agent can be combined in the solid formulation with another active agent described herein (eg, color imparting agent, thickening agent, oxidizing agent).
In some embodiments, the active alkalizing agent (s) in the solid formulation consists of an alkalizing agent (s), that is, the formulation does not include other types of active agents described herein. .
Suitable alkaline agents include ammonia and ammonium derivatives (eg, ammonium salts), organic amines, alkali and alkaline earth metal hydroxides, carbonates, carbamates, amino acids, and mixtures thereof.
Appropriate alkaline agents for use in accordance with some embodiments of the invention include but are not limited to an alkanolamine, a basic amino acid, a carbonate salt, a carbamate salt, a hydroxide salt, a silicate salt, and any combination of the themselves.
Examples of suitable alkanolamines include monoalkanolamines, dialkanolamines, trialkanolamines, monoalkyl monoalkanol amines, monoalkyl dialkanol amines and dialkyl monoalkanol amines, for example alkanolamines, di- (C14 alkanol) amines, tri- (C 1-4 alkanol) amines, mono ( C1-4 alkyl) -mono (C1-4 alkanol) -amines, mono (C1-4 alkyl) -di (C1-4 alkanol) -amines and di (C1-4 alkyl) -mono (C1-4 alkanol) - amines (e.g. monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), dimethyl MEA, aminobutanol, aminoethyl propanediol, aminomethyl propanediol, bis-hydroxyethyl tromethamine, diethylethanolamine, diisopropanolamine, dimethylamino methiIpropanol, isopropanolamine, methylethanolamine,
ES 2 823 977 T3 mixed isopropanolamines, triisopropanolamine, tromethamine);
Examples of suitable hydroxide salts include alkali metal hydroxides (eg, sodium or potassium hydroxide), alkaline earth metal hydroxides (eg, magnesium or calcium hydroxide), and ammonium hydroxide.
Examples of suitable carbonate salts include ammonium, alkali metal and alkaline earth metal carbonates such as Na2CO3, NaHCOs, K2CO3, KHCO3, (NH4) 2CO3, NH4HCO3, CaCO3 and Ca (HCO3) 2);
Examples of suitable carbamate salts include ammonium carbamate;
Examples of appropriate basic amino acids include arginine. Usine, oxy-lysine and histidine. Oligopeptides that comprise basic amino acids and are generally basic can also be included.
Examples of suitable silicate salts include sodium silicate and sodium metasilicate.
Additional examples of alkaline agents that can be used in some embodiments include ammonia and alkaline ammonium salts (eg, ammonium hydroxide); alkylamines (including monoalkylamines, dialkylamines, and trialkylamines), for example alkylamines di- (Ci-4 alkyl) amines and tri- (Ci-4) amines (eg, ethylamine, triethylamine, dipropylamine); alkanediamines such as C 1-4 alkanediamines (eg 1,3 diaminopropane); polyalkylene polyamines, such as dimers, trimers, tetramers, oligomers, and polymers of the aforementioned alkanediamines (eg, diethylenetriamine) and heterocyclic amines (such as morpholine);
In some embodiments, alkaline agents include ammonium hydroxide, monoethanolamine (MEA), diethanolamine (DEA), arginine, ammonium carbonate, ammonium hydrogen carbonate, sodium hydroxide, or mixtures thereof.
The amount of the alkaline agent to be employed in the preparation of a coloring composition can vary over a wide range, depending on the particular alkaline agent employed and the type of coloring sought.
In some embodiments, the active agent (s) in a solid formulation comprise at least one oxidizing agent.
In some embodiments, the oxidizing agent can be formulated into the solid formulation as another active agent described herein (eg, color imparting agent, thickening agent, alkaline agent).
In some embodiments, the active agent (s) in a solid formulation consist of an oxidizing agent (s), that is, the formulation does not include other types of active agents described herein.
In some embodiments, the oxidizing agent is suitable to react with a dye intermediate (eg, dye precursor) to form a dye (eg, oxidation dye). Such an oxidizing agent can be used in combination with one or more dye intermediates described herein to prepare a coloring composition for coloring with an oxidation dye.
Suitable oxidizing agents include but are not limited to a peroxide, including hydrogen peroxide and derivatives (eg, salts and complexes) thereof (eg, sodium peroxide, urea peroxide, melanin peroxide, polyvinylpyrrolidone complexes, hydrogen peroxide ), alkyl peroxides and aryl peroxides; inorganic metal peroxide salts such as periodates and perbromates (eg, sodium periodate, sodium perbromate), inorganic per salt bleach such as perborates (eg, sodium, potassium, or ammonium perborate), percarbonates, perphosphates, persulfates (eg ammonium, potassium or sodium persulfate) and percarbamides and mixtures thereof.
In some embodiments, the oxidizing agent is suitable for bleaching hair, eg, human hair. Bleaching may comprise bleaching of a natural pigmentation. Such an oxidizing agent (also referred to as a bleaching agent) can be used to prepare a coloring composition that is a bleaching composition, that is, a composition that is intended to effect a color on a surface by bleaching the existing color (for example , natural pigmentation).
Oxidizing agents for use in the preparation of a bleaching composition are generally not used in combination with a color-imparting agent. Rather, a bleaching composition is prepared with at least one bleaching agent, for example, by using a tablet comprising a bleaching agent (e.g., as described herein) without a color-imparting agent.
Thus, in some embodiments, the active agent (s) in a solid formulation consist of at least one bleaching agent.
Examples of suitable bleaching agents include without limitation such persulfate (for example, persulfate 50
ES 2 823 977 T3 ammonium, potassium or sodium).
The amount of oxidizing agent appropriate for formulations according to embodiments of the invention will depend on the particular agent selected and the use of specific coloration (eg, bleaching and / or oxidation of a dye intermediate).
In some embodiments, the active agent (s) in a solid formulation comprise at least one thickening agent.
In some embodiments, the thickening agent can be combined in the solid formulation with another active agent described herein (eg, color imparting agent, oxidizing agent, alkaline agent).
In some embodiments, the active agent (s) in a solid formulation consist of a thickening agent (s), that is, the formulation does not include other types of active agents described herein.
Many compounds known in the art may be suitable to serve as a thickening agent for a coloring composition as described herein.
In some embodiments, the thickening agent is soluble in a solvent used for the coloring composition. Suitable solvents for the coloring composition are described elsewhere herein.
In some embodiments, the thickening agent is a polymer (eg, water soluble polymer).
Examples of suitable thickening agents for inclusion in some embodiments of the invention include without limitation alginate; cellulose derivatives, such as carboxymethyl cellulose, hydroxyalkyl cellulose, and methyl cellulose; gums (in modified or unmodified form) such as agar agar; locust bean gum; carrageenan gum, ghatti gum, guar gum, acacia gum, caraway gum, tragacanth gum, scleroglucan gum and xanthan gum, · fatty alcohols such as cetyl alcohol, oleyl alcohol and cetearyl alcohol; fatty acids such as oleic acid; pectin, starch, amylose, amylopectin, dextrin; paraffin oil, bentonite; silicic acid, magnesium phyllosilicate; polyacrylamide, poly (2-acrylamido-2-methylpropanesulfonic acid), an acrylate polymer, a polyquaternium, polyvinyl pyrrolidone, polyvinyl alcohol, polyoxypropylene tridecyl ether, and polyoxyethylene tridecyl ether.
It will be understood that the multiple polymer descriptions (as before) herein are intended to encompass copolymers of any two or more disclosed polymers.
Herein a polyquaternium is any compound (eg, polycationic polymer) designated as such according to the International Nomenclature for Cosmetic Ingredients (INCI).
Acrylate polymer herein includes polymers and copolymers of acrylic acid, methacrylic acid, and ethers thereof (eg, ethyl acrylate, methyl methacrylate), according to INCI nomenclature.
In some embodiments, the concentration of the thickening agent (s) in a tablet when uncoated is no more than 80 percent by weight. In some embodiments, the concentration of the thickening agent (s) in a tablet when uncoated is no more than 50 percent by weight. In some embodiments, the concentration of the thickening agent (s) in a tablet when uncoated is less than 20 percent by weight.
In some embodiments, the active agent in a solid formulation comprises a combination of different types of active agents described herein.
In some embodiments, the active agent comprises at least one color-imparting agent (eg, as described herein) and at least one alkaline agent (eg, as described herein).
In some embodiments, the active agent comprises at least one color-imparting agent (eg, as described herein) and at least one thickening agent (eg, as described herein).
In some embodiments, the active agent comprises at least one color-imparting agent (eg, as described herein) and at least one oxidizing agent (eg, as described herein).
In some embodiments, the active agent comprises at least one oxidizing agent (eg, as described herein) and at least one alkaline agent (eg, as described herein).
In some embodiments, the active agent comprises at least one oxidizing agent (e.g., as described
ES 2 823 977 T3 herein) and at least one thickening agent (eg, as described herein).
In some embodiments, the active agent comprises at least one alkaline agent (eg, as described herein) and at least one thickening agent (eg, as described herein).
In some embodiments, the active agent comprises at least one color-imparting agent (eg, as described herein) and at least one thickening agent (eg, as described herein) and at least one agent. alkaline (eg, as described herein).
In some embodiments, the active agent comprises at least one color-imparting agent (eg, as described herein) and at least one oxidizing agent (eg, as described herein) and at least one agent. alkaline (eg, as described herein).
In some embodiments, the active agent comprises at least one color-imparting agent (eg, as described herein) and at least one oxidizing agent (eg, as described herein) and at least one agent. thickener (eg, as described herein).
In some embodiments, the active agent comprises at least one thickening agent (eg, as described herein) and at least one oxidizing agent (eg, as described herein) and at least one alkaline agent ( for example, as described herein).
In some embodiments, the active agent comprises all types of active agent described herein, that is, at least one color-imparting agent (e.g., as described herein) and at least one oxidizing agent (e.g. example, as described herein) and at least one thickening agent (for example, as described herein) and at least one alkaline agent (for example, as described herein).
In order to enhance the benefit of providing an active agent in preparation of a coloring composition in some embodiments, the amount of the active agent (s) in a tablet described herein is approximately equal to or less than (for example, 1/2, 1/3, 1/4, 1/5, 1/10, 1/20, 1/50), the lowest amount of the active agent (s) likely to be necessary for a coloring composition, an amount appropriate for treatment (for example, coloring) of a person's hair.
Consequently, an appropriate amount of active agent can be obtained from an integral number of such tablets (eg, about 2, 3, 4, 5, 10, 20, 50, 100, 150 or 200 tablets).
In some embodiments, the amount of the active agent in a tablet is sufficient such that no more than 100 tablets comprising a color-imparting agent (s) are needed to prepare a coloring composition, for example , a coloring composition sufficient to color the hair of at least one human head.
In some embodiments, the amount of the active agent in a tablet is sufficient such that no more than 150 tablets comprising a color-imparting agent (s) are needed to prepare a coloring composition, for example , a coloring composition sufficient to color the hair of at least one human head.
In some embodiments, the amount of the active agent in a tablet is sufficient such that no more than 100 tablets comprising an active agent described herein (for example, tablets comprising color-imparting agent (s) , oxidizing agent (s), alkalizing agent (s) and / or thickening agent (s) are necessary to prepare a coloring composition, for example a coloring composition wherein all the active agents of the coloring composition (for example, color imparting agent (s), oxidizing agent (s), alkalizing agent (s) and / or thickening agent (s)) are derived from tablets as described herein.
In some embodiments, the amount of the active agent in a tablet is sufficient such that no more than 150 tablets comprising an active agent described herein (tablets comprising color-imparting agent (s), agent ( s) oxidant (s), alkalizing agent (s) and / or thickening agent (s) are necessary to prepare a coloring composition (eg, as described herein).
In some embodiments, the water content of a solid formulation is less than 5 percent by weight of the total weight of a tablet when uncoated. In some embodiments, the water content of the solid formulation is less than 4 percent by weight. In exemplary embodiments, the water content of the solid formulation is less than 3 percent by weight. In some embodiments, the water content of the solid formulation is less than 2 percent by weight and in some embodiments, the water content of the solid formulation is even less than
ES 2 823 977 T3
1.5 percent by weight. The water content can optionally be obtained and / or determined as exemplified herein in the examples.
As illustrated in the examples section that follows, the present inventors have found that solid formulations as described herein with reduced water content (of less than 3 percent by weight or less than 2 percent by weight ) are advantageously characterized by improved stability due to the hygroscopic nature of some of the components (eg, the super-disintegrating agent).
In some embodiments, the solid formulation further comprises at least one excipient (eg, in addition to the active agent (s) and super-disintegrating agent (s) described herein). For example, binders and fillers are excipients included in some embodiments. Additional examples of excipients include a release agent, an anti-dandruff agent, an anti-foaming agent, antioxidant agents, a binder, a chelating agent, a conditioning agent, an emollient, an emulsifying agent, an exothermic compound, a filler, a fragrance, a free scrubber. radicals, a slip agent, a hair care agent, a humectant, a lubricant, an odor masking agent, an opacifying agent, an iridescent agent, pH adjusting agents, a plant extract, a preservative, a stabilizing agent, a Surfactant, a UV protective agent, a vitamin, a vitamin precursor, and a wetting agent.
In some embodiments, the excipient comprises a binder and / or filler. In some embodiments, the majority (> 50 weight percent) of the excipients in a solid formulation consist of a binder and / or filler.
In some embodiments, the total concentration of the binder and / or filler in a tablet when uncoated is at least 50 percent by weight. In some embodiments, the total concentration is at least 60 percent by weight. In some embodiments, the total concentration is at least 70 percent by weight. In some embodiments, the total concentration is at least 80 percent by weight.
A wide variety of water soluble and water insoluble binders can be used in tablets according to embodiments of the invention.
Suitable binders include proteins (such as gelatin); saccharides and their derivatives, including disaccharides (such as sucrose and lactose) and sugar alcohols (such as xylitol, sorbitol, and maltitol); polysaccharides and derivatives thereof (eg, starches, cellulose and / or modified cellulose); synthetic polymers such as polyvinyl pyrrolidone and polyethylene glycol (PEG); alginate and gums (eg gum acacia). Examples of suitable modified cellulose include microcrystalline cellulose and cellulose ethers such as hydroxypropyl cellulose (HPC).
Suitable fillers include but are not restricted to calcium phosphate (eg, dibasic calcium phosphate), calcium carbonate, silicic acid, and talc.
It will be appreciated that a particular excipient may fall into more than one of the categories mentioned above. For example, some compounds can be used both as binders to ensure the cohesiveness of the tablet and improve its mechanical strength and as fillers, commonly more inert, to provide a convenient dosage. Some of such compounds are still referred to in the art as binders-fillers. Similarly, some compounds may be considered non-stick (for example, compounds that reduce adhesion between a powder and tablet die faces to prevent sticking to tablet punches) or lubricants (for example, compounds that prevent ingredients from building up together. ). Similarly, some slip agents (for example, compounds that improve the flow of tablet ingredients to reduce friction and interparticle cohesion) can also act as anti-stick and / or lubricants.
Suitable non-sticks include but are not restricted to magnesium stearate.
Suitable slip agents include but are not restricted to calcium silicate, magnesium carbonate, magnesium silicon, silicon dioxide (including fumed silica and colloidal silicon dioxide), and talc (including colloidal talc).
Suitable lubricants include but are not restricted to common minerals such as talc or silica and fats, such as vegetable stearin, calcium stearate, magnesium stearate, sodium stearyl fumarate, and stearic acid.
Suitable anti-dandruff agents include pyroctone, olamine, zinc omadine, and climbazole.
Examples of suitable antifoam agents include silicones such as dimethylpolysiloxane and hydrated silica.
Suitable antioxidants include but are not restricted to ascorbic acid and its salts and derivatives (such as sodium ascorbate, erythorbic acid, ascorbyl palmitate, ascorbyl laurate), mercaptans and inorganic sulfites (such as sodium sulfite, sodium bisulfite, metabisulfite sodium, potassium sulfite and thioglycolic acid), butylated hydroxytoluene (BHT), butylated hydroxyanisole (BHA) and sodium dithionite. Such antioxidants may be
ES 2 823 977 T3 present in the tablets of the invention and / or in the appropriate medium up to 15 percent by weight. Commonly, such antioxidants can add up to 5% by weight of the final coloring formulation according to the invention.
Ascorbic acid is an exemplary excipient. Without being limited by any particular theory, it is believed that ascorbic acid advantageously and effectively acts as an antioxidant in tablets as described herein, while also reducing the designation time, as or exemplified herein. Exemplary concentrations of ascorbic acid range from 1 to 3 percent by weight.
Suitable surfactants include cosmetically acceptable anionic, cationic, zwitterionic and nonionic surfactants.
Suitable anionic surfactants include alkyl phosphate, alkyl carboxylate, alkyl sulfate, and alkyl sulfonate surfactants. Examples of suitable anionic surfactants include α-olefin sulfonate and its salts and alkali salts of sulfosuccinic acid half esters.
Examples of suitable cationic surfactants include long chain quaternary ammonium compounds, for example, behenyl trimethyl ammonium chloride, benzyl tetradecyl dimethyl ammonium chloride, cetyl pyridinium chloride, methyl trimethyl ammonium chloride, dimethyl tallow dihydrogen ammonium chloride, Dimethyl stearyl ammonium chloride, dimethyl stearyl benzyl ammonium chloride, Iauryl dimethyl benzyl ammonium chloride, Iauryl dimethyl ammonium chloride, stearyl trimethyl ammonium chloride, trimethyl acetyl ammonium bromide and tris- (oligooxy-ethyl) alkylammonium phosphate.
Examples of suitable zwitterionic surfactants include betaines (such as fatty acid amido alkyl betaine and sulfobetaine) and long chain alkyl amino acids (such as coco aminoacetate, coco amino propionate, sodium cocoamphopropionate, and sodium cocoamphoacetate).
Examples of suitable nonionic surfactants include polyethoxylated alcohols, polyethoxylated alkyl phenols, polyethoxylated glyceryl esters, and fatty acid derived polyethoxylated organic ethers.
In some embodiments, the concentration of such Surfactant is no more than 15 percent by weight.
Suitable emulsifying agents include but are not restricted to fatty acids (such as behenic acid, stearic acid, myristic acid, palmitic acid, and oleic acid) and anionic, cationic, zwitterionic, and nonionic surfactants (eg, as described herein. ).
In some embodiments, the concentration of such emulsifying agents is not more than 30 percent by weight.
A pH adjusting agent refers to acidifying agents and alkaline agents. Numerous suitable acidifying agents are known in the formulation art including but not limited to acetic acid, fumaric acid, hydrochloric acid, lactic acid, maleic acid, malic acid, nitric acid, phosphoric acid, propionic acid, monobasic sodium phosphate, sulfuric acid. and tartaric acid. Suitable alkaline agents include for example ammonium hydroxide, ammonium carbonate, diethanolamine, monoethanolamine, potassium hydroxide, sodium bicarbonate, sodium borate, sodium carbonate, sodium hydroxide, dibasic sodium phosphate and trolamine. Food acids and bases such as allantoin, bisabolol, pyrrolidonecarboxylic acids and salts thereof are also suitable.
It will be appreciated that an alkaline agent is used at considerably lower concentrations when used as a pH adjusting agent as described herein than when used as an active agent as described herein.
In some embodiments, the concentration of such pH adjusting agents is not more than 5 percent by weight.
Suitable chelating agents include but are not restricted to ethylenediaminetetraacetic acid (EDTA) and its salts such as disodium EDTA), ethylenediamine disuccinic acid (EDDS) and its salts, nitrilotriacetic acid (NTA), βalanindyacetic acid, phosphonic acids (such as etidronic acid ), pyrophosphates and zeolites.
In some embodiments, the concentration of such chelating agents is not more than 5 percent by weight.
Suitable fragrances include those from natural or synthetic sources. Natural fragrances include extracts and essential oils from flowers, stems, leaves, fruits, roots, woods, herbs, lawns, resins, balms, and raw animal ingredients (e.g., anise bergamot, cardamom, civet, myrrh, mace, patchouli, pine , rose, sandalwood and tarragon). Synthetic fragrances include ester, ether, aldehyde, ketone, alcohol, and hydrocarbon compounds (eg, benzyl acetate, benzyl ethyl ether, citronella, methyl cedar ketone, anethole, and terpenes).
In some embodiments, the concentration of such fragrances is no more than 5 percent by weight.
Suitable conditioning agents include but are not restricted to cationic surfactants (e.g., 54
ES 2 823 977 T3 as described herein), cationic polymers (for example, a polyquaternium), silicones (for example, silicone oil, cationic silicone, silicone gums, high refractive index silicone and resin resins). silicone), organic conditioning oils (e.g. hydrocarbon oils, polyolefins and fatty esters), alkylamidoamines, phospholipids (e.g. soy lecithin, Egg lecithin and cephalins) and quaternary compounds (eg cetrimonium chloride).
In some embodiments, the concentration of such conditioning agents is not more than 5 percent by weight.
Suitable humectants include water soluble liquid polyols (eg, glycerin, propylene glycol, hexylene glycol, butylene glycol, dipropylene glycol), polyalkylene glycols, urea, and mixtures thereof.
In some embodiments, the concentration of such humectants is not more than 30% by weight.
Suitable hair care agents include but are not restricted to betaine, cationic polymers (as described herein) or resins, cholesterol, lanolin derivatives, pantothenic acid, and vitamins.
Suitable vitamins include vitamins A, B3, B5, Be, C, E, F, and H and provitamins (vitamin precursors) thereof.
In some embodiments, the concentration of such hair care agents is no more than 5 percent by weight.
Suitable UV shielding agents include but are not restricted to derived benzophenones (such as uvinol), benzotriazole, cinnamic acid derivatives, coumarin, p-aminobenzoic acid, salicylic acid, and triazines.
In some embodiments, the concentration of such UV shielding agents is not more than 5 percent by weight.
Appropriate preservatives (in addition to antioxidants) include antimicrobial agents that prevent and / or retard bacterial growth and thus protect cosmetic products from deterioration.
Suitable iridescent agents include compounds such as ethylene glycol mono stearate and ethylene glycol distearate and PEG-3 distearate.
In some embodiments, the concentration of such iridescent agents is not more than 10 percent by weight.
An exothermic compound refers herein to a compound that releases heat on contact with a medium in which the tablet disintegrates (eg, to prepare a coloring composition). Examples of exothermic compounds suitable for inclusion in a solid formulation include but are not restricted to calcium chloride, calcium oxide, sodium acetate, and combinations thereof.
In some embodiments, the disintegration of the tablet is enhanced by the heat released by the exothermic compound. In such embodiments, the exothermic compound can be considered an auxiliary disintegration agent.
In some embodiments, the solid formulation comprises microcrystalline cellulose in a concentration ranging from 57 to 70 percent by weight. Avicel® PH-200 is an exemplary microcrystalline cellulose.
In some embodiments, the solid formulation comprises lactose (eg, spray dried lactose) in a concentration ranging from 21 to 27 percent by weight. SuperTab® 11SD is an exemplary lactose.
In some embodiments, the solid formulation comprises croscarmellose (eg, croscarmellose sodium) in a concentration ranging from 1.75 to 3.25 percent by weight (eg, 2 percent by weight or 3 percent by weight. ). AC-Di-Sol® SD711 is an exemplary croscarmellose.
In some embodiments, the solid formulation comprises magnesium stearate in a concentration ranging from 0.75 to 3.25 percent by weight (eg, 1 percent by weight or 3 percent by weight).
In some embodiments, the solid formulation comprises ascorbic acid in a concentration ranging from 0.75 to 1.25 percent by weight. In exemplary embodiments, the concentration is about 1 percent by weight.
In exemplary embodiments, the solid formulation consists of at least one color-imparting agent and excipients consisting of microcrystalline cellulose in a concentration in a range of 57 to 70 percent by weight, spray-dried lactose in a concentration in a range of 21 at 27 percent by weight, croscarmellose in a
ES 2 823 977 T3 concentration in a range of 1.75 to 3.25 percent by weight, magnesium stearate in a concentration in a range of 0.75 to 3.25 percent by weight and ascorbic acid in a concentration in a range of 0.75 to 1.25 percent by weight.
In some embodiments, the concentration of microcrystalline cellulose and lactose are roughly correlated, such that the concentration of both microcrystalline cellulose and lactose is relatively high when the total concentration of other ingredients is relatively low, and vice versa. In some embodiments, the lactose concentration is between 35.0% by weight and 39.0% by weight of the microcrystalline cellulose concentration. In some embodiments, the lactose concentration is between 36.0% and 38.2% of the microcrystalline cellulose concentration. In some embodiments, the lactose concentration is between 37.6% and 38.1% of the microcrystalline cellulose concentration.
In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the aforementioned excipients) consists of toluene-2,5-diamine, m-aminophenol, and resorcinol, agents that impart a natural tone. Toluene-2,5-diamine sulfate is an exemplary form of toluene-2,5-diamine. In exemplary embodiments, the concentration of toluene-2,5-diamine (e.g., toluene-2,5-diamine sulfate) in a tablet when uncoated is about 9.93 percent by weight, the concentration of m- aminophenol is about 0.91 weight percent and resorcinol concentration is about 4.05 weight percent.
In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the excipients mentioned above) consists of 2-amino-6-chloro-4-nitrophenol, the agent confers a golden hue. In exemplary embodiments, the concentration of 2-amino-6-chloro-4-nitrophenol in a tablet when uncoated is about 1.55 percent by weight.
In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the aforementioned excipients) consists of 4-amino-m-cresol, 4-amino-2- hydroxytoluene and 2-amino-6-chloro-4-nitrophenol, the agents impart an orange hue. In exemplary embodiments, the concentration of 4-amino-m-cresol in a tablet when uncoated is about 0.43 percent by weight, the concentration of 4-amino-2-hydroxytoluene is about 0.43 weight percent and the 2-amino6-chloro-4-nitrophenol concentration is about 11.7 weight percent.
In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the aforementioned excipients) consists of 1-hydroxyethyl-4,5-diaminopyrazole, 4-amino- 2hydroxytoluene and HC Red # 10 and 11, the agents impart a red hue. 1-Hydroxyethyl-4,5-diaminopyrazole sulfate is an exemplary form of 1-hydroxyethyl-4,5-diaminopyrazole. In exemplary embodiments, the concentration of 1-hydroxyethyl-4,5-diaminopyrazole (eg, 1-hydroxyethyl-4,5-diaminopyrazole sulfate) in a tablet when uncoated is about 6.3 percent by weight, the 4-amino-2-hydroxytoluene concentration is about 3.3 weight percent and HC Red # 10 and 11 concentration is about 0.075 weight percent.
In some embodiments, the color-imparting agent (s) in a tablet (eg, a tablet comprising the aforementioned excipients) consists of N, N-bis (2-hydroxyethyl) -p-phenylenediamine and 4-amino2-hydroxytoluene agents impart a violet hue. 1 N, N-bis (2-hydroxyethyl) -p-phenylenediamine sulfate is an exemplary form of N, N-bis (2-hydroxyethyl) -p-phenylenediamine. In exemplary embodiments, the concentration of N, N-bis (2-hydroxyethyl) -p-phenylenediamine (eg, N, N-bis (2-hydroxyethyl) -p-phenylenediamine sulfate) in a tablet when uncoated is around of 9.25 weight percent and the 4-amino-2-hydroxytoluene concentration is about 3.9 weight percent.
In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the excipients mentioned above) consists of toluene-2,5-diamine and 2,4-diamino-phenoxyethanol. and hydroxyethyl-3,4-methylene-dioxyaniline, the agents impart an ash hue. Toluene-2,5-diamine sulfate is an exemplary form of toluene-2,5-diamine. 2,4-Diamino-phenoxyethanol hydrochloride is an exemplary form of 2,4-diamino-phenoxyethanol. Hydroxyethyl-3,4-methylenedioxyaniline hydrochloride is an exemplary form of hydroxyethyl-3,4-methylene-dioxyaniline. In exemplary embodiments, the concentration of toluene-2,5-diamine (e.g., toluene-2,5-diamine sulfate) in a tablet when uncoated is about 0.24 percent by weight and the concentration of 2,4-Diamino-phenoxyethanol (for example, 2,4-diamino-phenoxyethanol dihydrochloride) is about 0.2 percent by weight and the concentration of hydroxyethyl-3,4-methylene-dioxyaniline (hydroxyethyl-hydrochloride) 3,4 methylenedioxyaniline) is about 0.46 percent by weight.
In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the excipients mentioned above) consist of p-aminophenyl and 4-amino-2-hydroxytoluene, the agents they give a pinkish hue. In exemplary embodiments, the concentration of p-aminophenol in a tablet when uncoated is about 0.35 percent by weight, the concentration of 4-amino-2-hydroxytoluene is about 0.45 percent by weight. .
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In some embodiments, the color-imparting agent (s) in a tablet (for example, a tablet comprising the aforementioned excipients) consists of toluene-2,5-diamine, hydroxyethyl-3,4- Methylenedioxyaniline, HC Yellow # 13, 2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine, and HC Blue # 15, the agents impart a green hue. Toluene-2,5-diamine sulfate is an exemplary form of toluene-2,5-diamine. Hydroxyethyl-3,4-methylene-dioxyaniline dihydrochloride is an exemplary form of hydroxyethyl-3,4-methylene-dioxyaniline. In exemplary embodiments, a concentration of toluene-2,5-diamine (e.g., toluene-2,5-diamine sulfate) in a tablet when uncoated is about 3.46 percent by weight, the concentration of hydroxyethyl-3,4-methylene-dioxyaniline (for example, hydroxyethyl-3,4-methylene-dioxyaniline hydrochloride) is around 3.43 weight percent, HC yellow # 13 concentration is around 2 percent by weight, 2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine concentration is around 0.025 weight percent and HC Blue # 15 concentration is around 0.25 weight percent .
In some embodiments, the color-imparting agent (s) in a tablet (eg, a tablet comprising the aforementioned excipients) consists of N, N-bis (2-hydroxyethyl) -p-phenylenediamine , 2,4-diamino-phenoxyethanol and HC Blue # 14 agents impart a blue hue. 1 N, N-bis (2-hydroxyethyl) -pphenylenediamine sulfate is an exemplary form of N, N-bis (2-hydroxyethyl) -p-phenylenediamine. 2,4-Diaminophenoxyethanol dihydrochloride is an exemplary form of 2,4-diamino-phenoxyethanol. In exemplary embodiments, the concentration of N, N-bis (2-hydroxyethyl) -p-phenylenediamine (eg, N, N-bis (2-hydroxyethyl) -p-phenylenediamine sulfate) in a tablet when uncoated is of about 6.2 percent by weight and the concentration of 2,4-diaminophenoxyethanol (for example 2,4-diamino-phenoxyethanol dihydrochloride) is about 5.05 percent by weight and the concentration of HC blue n 15 is about 0.2 percent by weight.
In some embodiments, a staining composition, kit, device, and / or method as described herein utilizes some or all of the tablets mentioned above, such that the natural, gold, orange, red, violet, ash tones, Pink, green and / or blue mentioned above serve as basic shades.
In some embodiments, the solid formulations described herein are packaged in individual low water transmission packages in order to minimize exposure to atmospheric moisture.
Coated formulations:
In some embodiments, the board further comprises a coating. Thus, in some embodiments, a solid formulation as described herein comprises a coated tablet.
As exemplified herein, a coating can surprisingly be beneficial to rapidly disintegrating tablets as disclosed herein, although a coating can slow down the disintegration rate of the tablet.
The coating may have advantageous properties, such as but not necessarily protective tablet ingredients (for example, by reducing or preventing its exposure to moisture, atmospheric oxygen and / or UV light) and / or improving the mechanical strength of the tablet (for example , by reducing friableness and / or increasing its hardness).
Thus, in some embodiments, the coating increases the shelf life of the tablet.
In some embodiments, coating dusting, dust reduction can result in a safer working environment.
Appropriate coatings can optionally be selected to retain some permeability such that a solvent of a medium that triggers disintegration (eg, permeability to water), which prevents degradation from premature moisture.
Suitable coating materials include but are not restricted to polymer and copolymer coatings such as carboxymethylcellulose (CMC), ethyl cellulose (EC), hydroxypropylcellulose (HPC), hydroxypropyl methylcellulose (HPMC), methyl hydroxyethyl cellulose (MHEC), polyethylene glycol (MHEC) ), polyvinyl alcohol (PvA), Polyvinylpyrrolidone (PVP), copolymers thereof (eg, polyvinyl alcohol-polyethylene glycol (PVA: PEG) copolymer). Certain sugar-based coatings (eg, xanthan: sugar) that provide similar properties may also be appropriate.
Exemplary coating materials include PEG, PVA, PVA: PEG copolymer, HPMC, and xanthan: sugar.
In exemplary embodiments, the coating consists of polyvinyl alcohol and a pigment (eg, a synthetic pigment). IR Kollicoat® Coating Polymer is an exemplary polyvinyl alcohol. Exemplary pigments include pigment green 7 (CAS # 1328-45-6) and pigment yellow 73 (CAS # 13515-40-7). An exemplary concentration of polyvinyl alcohol in the coating is about 80 percent by weight with the remainder being pigment.
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In exemplary embodiments, such a coating is obtained using a coating solution that consists of the coating materials of about 95 percent by weight in water (e.g., about 4 percent by weight in polyvinyl alcohol and about 1 percent by weight in polyvinyl alcohol. weight percent pigment).
The coating can comprise at least one excipient described herein. It will be appreciated that a coating is a logical location for certain types of excipients (eg, UV shielding agents).
In some embodiments, the thickness (that is, average thickness) of the coating is in a range of 1 µm to 100 µm. In some embodiments, the average thickness of the coating is in a range of 5 µm to 50 µm. In some embodiments, the average thickness of the coating is in a range of 10 µm to about 40 µm.
In some embodiments, the coating weight of the tablet is in a range of 0.1 to 10 percent by weight of the tablet when uncoated. In some embodiments, the weight of the tablet coating is in a range of 1 to 5 percent by weight of the tablet when uncoated. In some embodiments, the coating weight of the tablet is in a range of 1.5 to 3.5 percent by weight of the tablet when uncoated.
In some embodiments, the coating comprises at least one coloring agent. The coloring agent can be a color-imparting agent described herein (eg, a direct dye) or a coloring agent that is not particularly suitable for preparing a coloring composition.
Since the coating represents a small percentage of the solid formulation, such a coloring agent in a coating will not necessarily affect the color imparted by the coloring composition formed using the solid formulation.
Thus, for example, in some embodiments, the coating coloring agent and / or coating color may be a different color from the color imparted by the color-imparting agent (s) of a tablet.
In some embodiments, the coating coloring agent (and / or the coating color obtained with such a coloring agent) is an indicator of the coloring agent (s), if present in a tablet. For example, the color of the coating may be substantially the same as the color imparted by color-imparting agents on the tablet, and / or a particular color (eg, a light color) of the coating may be indicative of a tablet without an agent. color-imparting (eg, a tablet comprising a bleaching agent).
In some embodiments, the coating of the tablet allows the immediate initiation of disintegration of the tablet after contact with an appropriate medium.
In some embodiments, the tablet coating provides control over timing of disintegration, for example by providing delayed disintegration. In some embodiments, such a tablet is suitable for use in combination with at least one immediately disintegrating tablet, such that such tablets can be disintegrated in a predetermined sequence. For example, selection of appropriate coatings may allow tablets comprising color-imparting agent (s) and / or oxidizing agent (s) to disintegrate rapidly in a medium, while tablets comprising agent ( s) alkalizing agent (s) and / or thickening agent (s) are later disintegrated in the same medium.
In another example, delayed thickening of the medium can be obtained by using thinning tablets wherein the viscosity modifying agent is released into a non-viscous preform which is later activated to its viscous form using a delayed disintegration alkalizing tablet. Activation can be by providing an appropriate pH for thickening of the medium, in addition to the pH of the coloring process.
Solid formulation hardness is a measure of mechanical strength measured as fracture compression pressure that can be measured, for example, using standard industrial tablet hardness testing machines.
In some embodiments, the hardness of the solid formulation is selected to be appropriate for one or more intended purposes of the formulation, which may include for example: a) sustaining coating conditions; b) sustain handling and storage conditions; c) sustain supply conditions; and / or d) allow unbundling.
Therefore, the increase or decrease in hardness values between subsequent stages of the manufacturing process to the end use may be acceptable, as long as the hardness in each stage serves its purpose and the final hardness of the tablet at the point of use is compatible. with the selected conditions (for example, delivery conditions).
ES 2 823 977 T3
In some embodiments, the hardness of the tablet when uncoated which is sufficient to prevent undesirable tablet fracture and withstand the coating process (if the tablet is coated) is at least 1.0 kgf. In some embodiments, the hardness of an uncoated tablet is in a range of 1.0 kgf to 6.0 kgf. In some embodiments, the hardness of the uncoated tablet is in a range of 3.0 kgf to 5.0 kgf.
Without being limited by any particular theory, it is believed that excessively high hardness of a tablet when uncoated may be associated with low porosity, which can be detrimental to tablet disintegration.
In embodiments, where the tablets are not further coated, the hardness of the uncoated tablets must be compatible with their handling, storage and subsequent supply.
In embodiments where tablets are coated, the hardness after coating is related to the hardness of the tablet before coating and depends on a variety of factors including, for example, the type of coating, the thickness of the coating, the storage conditions. and the duration of storage.
In some embodiments, the hardness of the uncoated tablet is in the range of 2.0 kgf to 8.0 kgf.
Solid Formulation Properties:
The solid formulations described herein can be characterized by a short disintegration time, for example, in deionized water and / or an aqueous hydrogen peroxide solution. The measurement of disintegration times can be carried out as described in the examples section.
In some embodiments, the disintegration time of a solid formulation in deionized water is no more than 3 minutes. In some embodiments, the disintegration time of a solid formulation in deionized water is no more than 2 minutes. In some embodiments, the disintegration time of a solid formulation in deionized water is not more than 1 minute and can still last a few seconds (eg, 3 to 30 seconds).
In some embodiments, the disintegration time of a solid formulation in an aqueous hydrogen peroxide solution (9%) is not more than 5 minutes. In some embodiments, the disintegration time of a solid formulation in an aqueous hydrogen peroxide solution (9%) is not more than 4 minutes. In some embodiments, the disintegration time of a solid formulation in an aqueous hydrogen peroxide solution (9%) is not more than 3 minutes.
In some embodiments, exemplary solid formulations as described herein disintegrate in an aqueous hydrogen peroxide solution (6%) within seconds (see Figures 9A-B).
In some embodiments, the brittleness of the tablet (determined as described herein) is not more than 0.5%. In some embodiments, the brittleness of the tablet (determined as described herein) is not more than 0.37%.
Herein, the brittleness of tablets is determined by measuring weight loss after rotating the tablets 25 times at a speed of 25 rotations per minute, using a friable tester (e.g., a Thermonik Campbell apparatus. Electronics FTA-20), as described in the examples section herein.
In some embodiments, the tablets exhibit an increase in weight of less than 3% after storage for one month in open air, at a relative humidity of 52% and a temperature of 22.8 ° C. In some embodiments, the tablets exhibit an increase in weight of less than 2%.
In some embodiments, where the tablet comprises a coating and the coating has a color (eg, a color other than white), the coating color does not visibly fade after receiving 3 months of direct sunlight. In some embodiments, the coating color does not visibly fade after 6 months of direct sunlight.
Exposure to direct sunlight can be effected as described herein in the Examples Section. It will be understood that direct sunlight for a given period of time can be simulated, that is, exposure to an amount of light that is equivalent to direct sunlight for that period of time, as exemplified herein. .
As used herein, "visibly fading" refers to the fading that is noticeable to an average human observer.
ES 2 823 977 T3
As exemplified herein, the tablets described herein remain substantially free from microbiological contamination for at least 3 weeks, at least 10 weeks, and even at least 24 weeks, when stored under appropriate (but not particularly demanding) conditions. (eg, anhydrous conditions).
Thus, in some embodiments, the solid formulation tablets are substantially free from microbiological contamination, eg, microbiological contamination is at a level of less than 10 colony forming units / gram of the formulation.
The number of colony forming units can be determined as described in the examples section herein.
In some embodiments, tablets exhibit at least two of the aforementioned properties (i.e., a disintegration time in water as described herein, a disintegration time in aqueous hydrogen peroxide as described herein, a crumbly as described herein, a minimal weight increase in storage as described herein, a coating color stability as described herein, and / or an absence of microbiological contamination as described herein). In some embodiments, the tablets exhibit at least three of the aforementioned properties. In some embodiments, the tablets exhibit at least four of the aforementioned properties. In some embodiments, the tablets exhibit at least five of the aforementioned properties. In some embodiments, the tablets exhibit all of the six properties mentioned above.
For example, a disintegrating tablet comprising an alkaline agent, oxidizing agent, and / or thickening agent may consist largely of an active agent therein, in anhydrous form, if the active agent exhibits appropriate properties (eg, solubility). Thus, the active agent may comprise at least 50 weight percent, at least 60 weight percent, at least 70 weight percent, at least 80 weight percent, at least 90 weight percent, and still 100 percent by weight of such a tablet.
In some embodiments, a disintegrating tablet is prepared from ammonium carbonate and / or ammonium bicarbonate (alkaline agent).
In some embodiments, the disintegrating tablet is prepared from silicic acid (thickening agent).
In some embodiments, the disintegrating tablet is prepared from an oxidizing salt such as a periodate, a perbromate, a perborate, a percarbonate, a perphosphate, a persulfate, and / or a percarbamide (oxidizing agents).
In some embodiments, the solid formulation is suitable for use in coloring human hair, for example, being suitable for preparing a coloring composition suitable for coloring human hair or hair.
In such formulations, the ingredients are selected to be cosmetically acceptable, at least in the amounts used in such a coloring composition. The acceptability of ingredients can easily be determined by those of skill in the cosmetic arts, for example, based on determinations of a regulatory agency and such information is regularly updated.
When intended for human use, the color-imparting agents and the other ingredients or additives in the compositions described herein must satisfy the safety requirements applicable to such cosmetic products. In particular, the ingredients are selected for their compatibility with each other and for their lack of toxicity to the hair and scalp. Where applicable, the constituents of the tablet or media can be salt or solvate derivatives of the parent compounds listed above and for example, the color-imparting agents can be used in the form of cosmetically acceptable salts or solvates of the original dye.
The term "cosmetically acceptable," as used herein, refers to constituent ingredients, including color-imparting agents, their salts and / or solvates, that are safe and effective for topical use in mammals, particularly humans, and that possess or are compatible with the desired coloring activity, are considered safe and do not cause toxicity, irritation, allergic reaction and the like. Such regulatory information is updated from time to time and is readily available.
Cosmetically acceptable salts include salts of acidic or basic groups. Cosmetically acceptable acid addition salts include, but are not limited to, hydrochloride, hydrobromide, hydroiodide, nitrate, sulfate, bisulfate, phosphate, acid phosphate, isonicotinate, acetate, Iactate, Salicylate, citrate, tartrate, pantothenate, bitartrate, ascorbate, succinate, maleate, gentisinate, fumarate, gluconate, glucaronate, saccharate, formate, benzoate, glutamate, methanesulfonate, ethanesulfonate, benzenesulfonate, p-toluenesulfonate, and pamoate salts. Certain compounds of the invention can form cosmetically acceptable salts with various amino acids . Appropriate basic salts
ES 2 823 977 T3 include, but are not limited to, aluminum, calcium, lithium, magnesium, potassium, sodium, zinc and diethanolamine salts. Cosmetically acceptable solvates include, but are not limited to, hydrates, ethanolates, and methanolates.
Since a solid formulation must be suitable for preparing a coloring composition, it will be appreciated that the ingredients of a solid formulation, as a whole, must be suitable for preparing a given coloring composition, for example, a composition comprising a particular medium. (for example, a solvent, a cream, a gel). Thus, in some embodiments, all of the ingredients are selected to be appropriate for use in combination with the same medium of a coloring composition.
Process to prepare solid formulations:
Solid formulations as described herein can be prepared into a tablet by compression techniques.
Hence, in accordance with another aspect of embodiments of the invention, there is provided a method for preparing a solid formulation described herein. The method comprises forming a mixture comprising at least one super-disintegrant and at least one active agent to be included in the solid formulation (eg, as described herein); and compressing the mixture to thereby form the tablet described herein. In some embodiments, the blend comprises all ingredients to be included in the tablet when uncoated (eg, ingredients described herein).
For example, in direct compression tableting, a measured volume of a blend fills a mold, then a lower punch and an upper punch uniaxially compress the blend into the mold.
In some embodiments, the ingredients or a portion of the ingredients are provided as anhydrous powders.
In some embodiments, the ingredients or a portion of the ingredients are ground and / or granulated before being mixed and compressed to form the tablets described herein. The tablet ingredients can be granulated by any granulation method known in the art. In some embodiments, granulation is by anhydrous granulation.
As is known in the art of tablet pressing, it is advantageous for all ingredients to be both uniform in overall density to avoid segregation of ingredients during the tabletting process. When the ingredients have similar material densities, the approximate size uniformity of the ingredient particles ensures that homogeneous concentrations and doses are delivered with each tablet. In some embodiments, such approximate size uniformity is obtained by milling (eg, by blade milling, hammer milling, etc.) and / or by sieving.
In some embodiments, the ingredients are provided as free-flowing powders, for example, in order to ensure uniform tablet weight.
In some embodiments, the size of the particles in the mixture is generally less than 200 µm. Thus, in some embodiments, at least 70 percent by weight of the particles in the mixture have a diameter of 200 µm or less. In some embodiments, at least 80 percent of the particles in the mixture have a diameter of 200 µm or less. In some embodiments, at least 90 percent by weight of the particles in the mixture have a diameter of 200 µm or less.
In some embodiments, the size of the particles in the mixture is generally in a range of 20 µm to 150 µm. Thus, in some embodiments, at least 70 percent by weight of the particles in the mixture have a diameter in a range of 20 µm to 150 µm. In some embodiments, at least 80 percent by weight of the particles in the mixture have a diameter in a range of 20 µm to 150 µm. In some embodiments, at least 90 percent by weight of the particles in the mixture have a diameter in the range of 20 µm to 150 µm.
In some embodiments, the size of the particles in the mixture is generally in a range of 40 µm to 120 µm. Thus, in some embodiments, at least 70 percent by weight of the particles in the mixture have a diameter in the range of 40 µm to 120 µm. In some embodiments, at least 80 percent by weight of the particles in the mixture have a diameter of 40 µm to 120 µm. In some embodiments, at least 90 percent by weight of the particles in the mixture have a diameter in a range of 40 µm to 120 µm.
In some embodiments, the particle size of the coloring agent in the mixture is generally less than 200 µm. Thus, in some embodiments, at least 70 percent by weight of the color-imparting agent particles in the mixture have a diameter of 200 µm or less. In some embodiments, at least 80 percent by weight of the color-imparting agent particles in the mixture have a diameter of 200 µm or less. In some embodiments, at least 90 percent by weight of the color-imparting agent particles in the mixture have a diameter of 200 µm or less.
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In some embodiments, the particle size of the color-imparting agent in the mixture is generally in a range of 20 µm to 150 µm. Thus, in some embodiments, at least 70 percent by weight of the color-imparting agent particles in the mixture have a diameter in the range of 20 µm to 150 µm. In some embodiments, at least 80 percent by weight of the color-imparting agent particles in the mixture have a diameter in a range of 20 µm to 150 µm. In some embodiments, at least 90 percent by weight of the color-imparting agent particles in the mixture have a diameter in the range of 20 µm to 150 µm.
In some embodiments, the size of the color-imparting agent particles in the mixture is generally in a range of 40 µm to 120 µm. Thus, in some embodiments, at least 70 percent by weight of the color-imparting agent particles in the mixture have a diameter in the range of 40 µm to 12 0 µm. In some embodiments, at least 80 percent by weight of the color imparting agent particles in the mixture have a diameter in the range of 40 µm to 12 0 µm. In some embodiments, at least 90 percent by weight of the color-imparting agent particles in the mixture have a diameter in the range of 40 µm to 120 µm.
Some ingredients may be commercially available as particles within a desired size range. Others can optionally be screened to reduce the amount of the undersized or oversized particles. If necessary, certain ingredients can optionally be pre-milled with any suitable milling machine available and optionally further sieved to obtain the desired uniformity. The ingredients, whether or not ground and / or sieved, can optionally then be mixed to form an appropriate mixture for the manufacture of homogeneous formulations. Certain ingredients may be subject to safety regulations and any process using such ingredients must be carried out with all due care. For example, some color-imparting agents can be toxic if inhaled and must be handled in accordance with any process that involves dust formation.
In some embodiments, the process or processes involved in the preparation of tablets according to the invention are carried out under anhydrous conditions. In some embodiments, the anhydrous conditions comprise a relative humidity of less than 20%. In some embodiments, anhydrous conditions comprise a relative humidity of less than 10%. In some embodiments, anhydrous conditions comprise a relative humidity of less than 5%. In some embodiments, the anhydrous conditions comprise a relative humidity of less than 2%.
In general, the higher the pressure applied during compression, the harder the tablet produced. As discussed herein, the tablets described herein must be hard enough to provide the mechanical strength required to maintain their integrity, for example during manufacture, storage, transportation, and handling, as long as they are sufficiently friable. to allow its disintegration on contact with an appropriate medium. The compression pressure can optionally be controlled, for example, by the final closing distance between the punches.
In some embodiments, compression is effected under conditions (eg, compression pressure) that result in the tablet having a hardness described herein (for an uncoated tablet).
The geometry of the tablet is determined by the shape of the punches, the volume of the mold and the position of the punches relative to each other during compression.
In some embodiments, the aforementioned parameters are selected to provide a tablet geometry described herein.
In some embodiments, spheroidal tablets (eg, as described herein) are prepared by direct compression tableting using a modified ball tablet punch having a rounded concave punch shape and by selecting at a force / appropriate compression pressure. At a given compression pressure, a tablet thickness similar to the diameter of the punch can be obtained by providing tablets that are close to spherical in shape.
A lower compression pressure would be appropriate for the preparation of elongated capsules, while a higher compression pressure would be appropriate for the preparation of flat tablets.
In some embodiments, the process further comprises coating the tablet obtained by compression (eg, to obtain a coating described herein).
There are several suitable tablet coating methods known in the art, for example, dry coating, film coating, fluid bed coating, perforated and non-perforated tray coating, Wurster coating, solid wall tray coating, sugar coating. and top coating. Any method that can be used to coat an uncoated tablet described herein
ES 2 823 977 T3 document (for example, an uncoated tablet characterized by a hardness described herein) and would result in a coated tablet described herein (for example, a coated tablet characterized by a hardness described in the present document) is appropriate.
In some embodiments, the agents used to form coatings are suspended or dissolved in an appropriate liquid. Suitable liquids include water, polyhydric alcohols (such as ethylene glycol, propylene glycol, and glycerin), ethyl acetate, methylene dichloride, oils (including natural or synthetic oils, such as plant oils, paraffin oils, and silicone), and combinations thereof. . The selection of an appropriate solvent for suspending or dissolving a coating agent is within the capabilities of those skilled in the art of tablet coating.
In some embodiments, water is the predominant solvent for the liquid and other liquids (eg, alcohols, oils), if used, are in an amount sufficient to improve the miscibility of the coating agent.
In some embodiments, lower aliphatic alcohols (eg, methanol, ethanol, and propanol) and ketones (eg, acetone and butanone) are used as the solvent.
An exemplary coating method for tablets of the invention comprises spray coating using a perforated tray spray coating apparatus. In such a coating method, a spray gun (s) applies a coating to the tablets at a desired flow rate of the coating solution and the propellant gas pattern while the tray rotates, ensuring that the tablets are evenly coated.
In some embodiments, the tablets are concurrently dried by heated gas (usually air), eg, blown from an upper conduit through the tray exiting through the perforations in the tray.
The temperature of the heated air can optionally be controlled by an inlet gas temperature control. The temperature can optionally be monitored at the level of the exhaust duct under the product bed. In some embodiments, the tablets are assumed to be around the same temperature as measured in the exhaust.
In some embodiments, the quality of coating is improved by performing anti-dust formation and / or preheating steps of the tablet prior to the coating process previously described.
Without being limited by any particular theory, the perforated tray coating method described herein is believed to be advantageous due to a short exposure of the tablets to the coating solution, which is the result of continuous heating and drying. The short exposure is believed to improve the stability of the tablet core, especially of the reactive ingredients in it.
In exemplary embodiments, the process further comprises drying the tablet. In an exemplary embodiment, drying is carried out in a vacuum oven.
In some embodiments, drying is carried out at a temperature of 30-80 ° C (eg 40 ° C), under reduced pressure (eg 1.5 kPa (15 mbar)).
In some embodiments, drying is performed for a period of time of at least 10 hours (eg, about 20 hours).
Tablets can optionally be dried when coated or when uncoated. In an exemplary process, the coated tablets are dried.
As exemplified herein, drying (eg, as described herein) can reduce the water content of the tablet to less than 3 percent by weight and yet to less than 2 percent by weight or less. 1 percent by weight.
In some embodiments, the process further comprises sublimation (eg, freeze drying of tablet ingredients), which can optionally promote dissolution or disintegration.
Compositions:
The rapid disintegration tablets (both coated and uncoated) disclosed herein can advantageously be used to form compositions for treating hair. The composition can be, for example, a coloring composition or any composition useful in a hair coloring process, as defined herein.
ES 2 823 977 T3
According to another aspect of embodiments of the invention, a composition suitable for use in treating hair is provided. The composition comprises an aqueous medium and at least one of the solid formulations as described herein disaggregated in the medium.
As used herein, the phrase "aqueous medium" encompasses water, aqueous solutions, and aqueous suspensions.
As used herein, the phrase "aqueous solution" refers to a solution in which more than 50 percent by weight of the solvent consists of water. The remainder of the solvent can be, for example, a water-miscible cosolvent. Examples of suitable cosolvents in an aqueous solution include lower aliphatic alcohols (eg, ethanol, propanol, and isopropanol) and polyhydric alcohols (eg, ethylene glycol, propylene glycol, and glycerin) and combinations thereof.
As used herein, the phrase "aqueous suspension" refers to a suspension where the continuous phase is water or an aqueous solution (as defined herein). Examples of an aqueous suspension include oil-in-water emulsions (eg, creams), aqueous gels, and aqueous suspensions of surfactants (eg, Surfactant micelles in aqueous solution).
Examples of suitable oils for inclusion in aqueous media (eg, oil-in-water emulsions) include natural or synthetic oils, such as plant oils, paraffin oils, and silicone) and combinations thereof.
Examples of surfactants that can be included in aqueous media include soap (eg, ammonium or potassium oleate) and oxyethylenated nonionic surfactants (such as polyalkoxylated or polyglycerolated fatty alcohols).
The aqueous medium may further comprise at least one active agent described herein, that is, an active agent that is not derived from disintegration of a tablet.
In some embodiments, the aqueous medium comprises at least one oxidizing agent (eg, as described herein), such that the medium is an oxidizing medium.
In some embodiments, the aqueous medium comprises at least one alkaline agent (eg, as described herein), such that the medium is an alkalizing medium.
In some embodiments, the aqueous medium comprises at least one thickening agent (eg, as described herein), such that the medium is a thickening medium.
In some embodiments, the aqueous medium comprises at least one color-imparting agent (eg, as described herein), such that the medium is a color-imparting medium.
In some embodiments, the aqueous medium comprises at least one oxidizing agent (eg, as described herein) and at least one alkaline agent (eg, as described herein), such that the medium it is an oxidizing medium and an alkalizing medium.
In some embodiments, the aqueous medium comprises at least one oxidizing agent (eg, as described herein) and at least one thickening agent (eg, as described herein), such that the medium it is an oxidizing medium and a thickening medium.
In some embodiments, the aqueous medium comprises at least one alkaline agent (eg, as described herein) and at least one thickening agent, such that the medium is an alkalizing medium and a thickening medium.
In some embodiments, the aqueous medium comprises at least one oxidizing agent (eg, as described herein), at least one alkaline agent (eg, as described herein), and at least one thickening agent ( for example, as described herein).
In some embodiments, the composition comprises at least one color-imparting agent. Such a composition is referred to herein as a coloring composition. The color-imparting agent (s) may be a component of the aqueous medium (for example, a color-imparting medium) or a component of a solid formulation (for example, as described in present document).
In some embodiments, the solid formulation comprises at least one color-imparting agent as an active agent (eg, as described herein). In some embodiments, the composition further comprises at least one additional active agent that is an alkaline agent, oxidizing agent, and / or thickening agent (eg, as described herein). The alkalizing agent (s), oxidizing agent (s) and / or
ES 2 823 977 T3 thickening agent (s) may be a component of the aqueous medium (for example, an alkalizing medium, oxidizing medium and / or thickening medium described herein) and / or a component of a solid formulation (eg, as described herein).
In some embodiments, the composition comprises at least one solid formulation comprising at least one disintegrated color imparting agent in an aqueous medium comprising at least one additional active agent which is an alkaline agent, oxidizing agent, and / or thickening agent (e.g. , an alkalizing medium, oxidizing medium and / or thickening medium described herein).
In some embodiments, such a composition is suitable for use in coloring human hair (eg, as described herein).
Since the composition comprises a disintegrated solid formulation as described herein, it will be appreciated that the composition will comprise substantially all of the ingredients of the solid formulation (eg, excipients, super-disintegrating agents, disintegration aids), as described in This document.
The composition can be, for example, a composition prepared according to any method described hereinafter.
Each active agent in the composition can result from the breakdown of a solid formulation comprising that active agent (e.g., a solid formulation described herein) or be added to the composition from a different source, such as a solid (e.g. eg, a powder), a liquid medium (eg, a medium described herein), etc.
In some embodiments, the composition comprises a plurality of disintegrated tablets (eg, tablets comprising color imparting agent (s), tablets comprising oxidizing agent (s), tablets comprising alkalizing agent (s) (s), and / or tablets comprising thickening agent (s), the plurality of tablets customizing the hair coloring of an individual subject.
In some embodiments, the aqueous medium is customized for the coloring of an individual subject's hair. For example, the type of the active agent (s) in the aqueous medium and the concentration (s) thereof can be customized for an individual.
For example, tablets and / or media can be selected to take into account an individual's initial hair color, which can be affected by natural pigmentation, hair reflectance, previous coloring, and / or other chemical agents present in or on. the hair and the final color desired by the individual (for example, color-conferring agents are selected to obtain the desired color starting from the initial color; an individual's hair type (eg, European, Asian, African, etc .; straight, wavy, curly, or kinky; thin or thick; dry, normal, or oily); a desired type of coloring process, eg, permanent coloring, semi-permanent coloring, demi-permanent coloring, temporary coloring, and / or bleaching (eg, bleaching); and / or any sensitivities of an individual (eg, avoiding or minimizing components to which an individual is allergic or otherwise sensitive). Build based on an initial color and desired color can be accomplished based on an analysis of how to advance from an initial color to a desired color, as described herein (see, for example, Section I).
It will be appreciated that the aforementioned types of coloring process may use different types of color-imparting agent (if any), and / or amounts of alkaline agent, as described herein.
In some embodiments, the viscosity of the composition is appropriate to provide sufficient contact time between the composition and the fibers to be colored, as described herein.
Viscosity can depend on many components in the composition, including components in the aqueous medium and / or components in one or more disintegrated tablets.
In some embodiments, the viscosity is primarily determined by the amount of the thickening agent (s). In some embodiments, the thickening agent (s) is (are) released from a disintegrating tablet.
In some embodiments of the various aspects of embodiments of the invention (eg, methods, devices, kits described herein), a disintegrating tablet comprising an active agent described herein is not necessarily a disintegrating tablet. disintegrates in accordance with embodiments of the invention (eg, comprising a super disintegrating agent as described herein).
A coloring composition as described herein, or any other composition for treating hair as described herein, may have a final liquid form (for example, a
ES 2 823 977 T3 aqueous solution), a cream, a gel, a lotion, an emulsion, a paste or any other form acceptable in the field of hair coloring. The final form is determined as desired, with appropriate ingredients and concentrations thereof being selected (eg, a thickening agent).
Kits:
Solid formulations in tablet form, as described herein, are highly useful for hair coloring, particularly when different active agents described herein are used in combination, for example by using different solid formulations described herein. herein in order to provide some or all of the desirable active agents for coloring.
Furthermore, solid tablet formulations comprising at least one color-imparting agent, as described herein, are particularly useful in combinations comprising solid formulations with different color-imparting agents. Such tablets can then be combined to provide a desired coloring composition.
Thus, in another aspect of embodiments of the invention, a hair coloring kit is provided, the kit comprising a plurality of sets of a solid formulation described herein. Each set consists of a plurality of substantially identical tablets different in type of active agent and / or amount of active agent. Such sets may include, for example, one or more sets of tablets comprising at least one color-imparting agent, one or more sets of tablets comprising at least one oxidizing agent, one or more sets of tablets comprising at least one agent. alkaline and / or one or more sets of tablets comprising at least one thickening agent.
In some embodiments, at least a portion of the sets in the kit consist of solid formulations comprising at least one color-imparting agent (eg, as described herein).
In some embodiments, each of the sets in the kit consists of solid formulations comprising at least one color-imparting agent (eg, as described herein).
The color conferring agents in each set represent a basic shade, as defined herein.
In some embodiments, the kit comprises at least 3 basic shades. In some embodiments, the kit comprises at least 4 basic shades. In some embodiments, the kit comprises at least 5 basic shades. In some embodiments, the kit comprises at least 6 basic tones. In some embodiments, the kit comprises at least 7 basic tones. In some embodiments, the kit comprises at least 8 basic shades. In some embodiments, the kit comprises at least 10 basic shades. In some embodiments, the kit comprises at least 15 basic shades. In some embodiments, the kit comprises at least 20 basic shades.
In some embodiments, the number of basic tones in a kit is in a range of 3 to 36. In some embodiments, the number of basic tones in a kit is in a range of 3 to 24. In some embodiments, the number of tones basics in a kit is in a range of 6 to 18.
In some embodiments, the color-imparting agents of the different base shades in a kit are selected to be sufficiently different from each other to allow a large number of shades to be obtained by combining base shades in different proportions.
In some embodiments, the kit further comprises at least one set of solid formulations that does not comprise a color-imparting agent (eg, in addition to basic shades). Such set (s) may comprise, for example, at least one active agent other than the color-imparting agent (for example, alkalizing agent (s), oxidizing agent (s) and / or thickening agent (s)). In some embodiments, at least one set comprises an alkaline agent as an active agent. In some embodiments, the set comprising an alkaline agent in addition to one or more sets for basic tones, as described herein.
In some embodiments, the sets of solid formulations in a kit are customized to color the hair of an individual subject. The kit can be customized for a coloring process to be carried out by an individual (for example, a kit to color the hair once, or a kit to carry out the same coloring process multiple times), and / or for a plurality of different processes. coloring that can be performed by an individual (for example, a hair coloring kit multiple times).
For example, sets may be selected to take into account an individual's initial hair color (for example, basic shades may be deficient in shades close to the individual's hair color), which may be affected by natural pigmentation, hair reflectance, pre-coloring and / or other chemical agents present in or on the hair; the final color (s) desired by an individual (e.g. basic shades
ES 2 823 977 T3 may be biased towards shades preferred by the individual); an individual's hair type (eg, European, Asian, African, etc .; straight, wavy, curved, or kinky; thin or coarse; dry, normal, or oily); a desired type of coloring process (eg, permanent coloring, semi-permanent coloring, demi-permanent coloring, temporary coloring and / or bleaching); and / or any sensitivities of an individual (eg, avoiding or minimizing components to which an individual is allergic or otherwise sensitive). The making of the basic shades based on an initial color and a desired color can be carried out based on an analysis of how to advance from an initial color to a desired color, as described herein.
In some embodiments, the sets of solid formulations are selected to be universal, that is, they are intended to be as useful as possible to a wide variety of people with different needs (eg, needs as described herein).
In some embodiments, the kit includes written or otherwise readable instructions that describe how to obtain a desired color, for example, how to select basic shades and / or other active agents, how many tablets of each basic shade, and / or other agents. active ingredients include in a composition, how to mix the basic shades with other active agents (for example, tablets and / or media comprising active agents) and how to apply (for example, for how long to apply) the coloring composition obtained.
Such instructions may be in the form of color coordinates or may be provided to an individual after analyzing an individual's hair and converting the analysis to the desired color coordinates. In some embodiments, the analysis is done by means of an optical reader as described herein. In some embodiments, the determination of the coloring composition is done by algorithmic methods as described herein.
In some embodiments, the kit further comprises an appropriate means for preparing a coloring composition (eg, as described herein). The medium can optionally be included in the kit enclosed in a container. In some embodiments, the medium is an aqueous medium.
In some embodiments, the medium is an oxidizing medium (eg, an oxidizing medium described herein), that is, a medium comprising an oxidizing agent (eg, an oxidizing agent described herein). Such a medium is particularly suitable, for example, when the kit does not include solid formulations comprising such an oxidizing agent.
In some embodiments, the medium is an alkalizing medium (eg, an alkalizing medium described herein), that is, a medium comprising an alkaline agent (eg, an alkaline agent described herein). Such a medium is particularly suitable, for example, when the kit does not include solid formulations comprising such an alkaline agent.
In some embodiments, the medium is a color-imparting medium (eg, a color-imparting medium described herein), that is, a medium comprising at least one color-imparting agent (eg, agent (s) conferring color (s) described herein). Such a medium is particularly suitable, for example, when the kit does not include solid formulations comprising such color-imparting agent (s).
In some embodiments, the medium is a carrier medium, that is, a medium that does not comprise a substantial amount of an oxidizing agent, color-imparting agent, or alkaline agent. In some embodiments, the carrier medium does not comprise a substantial amount of any active agent described herein. In some such embodiments, the kit comprises solid formulations comprising oxidizing agent (s), color-imparting agent (s), and alkalizing agent (s).
In some embodiments, the medium is suitable for disintegration of the kit tablets (eg, all the tablets in the kit).
In some embodiments, the viscosity of the medium is selected to be appropriate to form a composition for coloring by disintegrating the tablets in the medium. In some embodiments, the aqueous medium in the kit has a viscosity of 1 poise or less (as measured at a shear rate of 10 s<sup>-1</sup> and a temperature of 25 ° C).
In some embodiments, an alkalizing medium, a color-imparting medium, and / or an oxidizing medium in a kit is in ready-to-use form, for example, with respect to the concentration of the active agent compatible with the type of coloration desired.
In some embodiments, an alkalizing medium, a color-imparting medium, and / or an oxidizing medium in a kit is provided as a high concentration concentrated solution, which can be diluted to a desired concentration with appropriate amounts of carrier medium. In some embodiments, such a carrier medium for dilution is included in the kit. In some embodiments, such a carrier medium for dilution is not included in the kit (e.g., where the
ES 2 823 977 T3 carrier medium for dilution is water).
The rapid disintegration tablets described herein, when used for the preparation of a (personalized) hair treatment composition, can be measured and when desired, mixed with appropriate means, to provide a desired composition, as described. described in this document. Selection of the type and amount of each active agent in the composition whether the active agent is in the form of a solid tablet formulation or in any other form, measurement of a desired amount and mixing can be done manually or automatically.
In most cases, automating desired sets of single-use personalized hair coloring formulas or tablet delivery at the point of purchase or point of use is advantageous. Automatic dispensing devices have several advantages. For example, automated delivery devices can provide increased control over dosing accuracy and reproducibility, can quickly prepare custom coloring preparations, and facilitate the introduction of computerized systems for color preparation.
The use of tablets instead of traditional wet forms is generally advantageous as it saves storage space, allows a cleaner work environment, and improves the dosing capacity of color-imparting agents, hence the accuracy and reproducibility of the coloring formulas. The space saving can be further increased by having the relevant media in the form of fast disintegrating tablets.
The use of coated tablets and their free-flowing nature facilitate their use within an automated or manual dispensing device during delivery. The use of coated tablets significantly reduces contact of coloring agents with internal portions of a dispensing device, minimizing contamination of such parts by pre-dispensed sets of coloring tablets, which can affect the accuracy of coloring formulas.
IV. The Dispensing Device:
The present inventors have designed a dispensing device to automatically deliver a desired set of tablet formulation, to thereby produce a hair treatment composition and / or kit.
Although tablet dispensers are known in the pharmaceutical field, none were designed to mix specific amounts of various types of tablets on a custom basis and therefore this particular problem was not previously addressed.
In some embodiments, the dispensing device is designed to be suitable for providing personalized compositions for treating hair and in some embodiments, for providing a personalized coloring composition (eg, hair coloring composition). The device is capable of dispensing different combinations and amounts of tablet formulations such as those described herein, which can optionally be used in combination with any additional media and / or agents as described herein to form a composition of coloration. The device may further be capable of dispensing both tablet formulations and liquid media or formulations to form the custom coloring composition.
According to one aspect of some embodiments of the present invention there is provided a device for preparing a composition for treating hair, as described herein, whereby the composition is formed from a plurality of tablets. The device is configured such that it comprises a plurality of containers or compartments, at least some of the compartments or containers have an appropriate outlet to deliver a solid formulation in the form of a tablet and a dispenser unit configured to deliver a predetermined quantity of tablets , the surviving compartments and the distributor unit are interconnectable.
Pluggable means that the containers and the dispenser unit are in communication in a manner that allows the tablets to flow out of the container and be subjected through the dispenser unit. The dispenser unit and the containers and / or compartments can be connected to each other either directly or indirectly.
Thus, the device according to embodiments of the present invention is configured to be suitable for dispensing tablets and may optionally be configured to deliver solid formulations in a different form of tablets (eg powder or granules) and / or to deliver liquid formulations. (for example, aqueous media or solutions), in addition to dispensing tablets.
In some embodiments, only a portion of the containers in the dispensing device are appropriate containers for holding and dispensing tablets. In some embodiments, all the vessels in the device
ES 2 823 977 T3 dispensers are suitable for containing and dispensing tablets.
Those containers that are configured appropriate to contain and dispense tablets are referred to herein as tablet containers.
In the following, the term container may refer to an individual separate container or to a single compartment within a multi-compartment container, unless otherwise clear from the context.
Tablet Containers:
In some embodiments, each of the containers or compartments in the dispensing device comprises a base, one or more walls, and a cap. Each individual container or compartment as described hereinafter further comprises a container outlet. The tablet containers further comprise an outlet that is configured to allow the tablets to be dispensed from the container. The outlet can be located on the container in any appropriate position for supply means (also referred to as a dispenser element). When the delivery involves gravitational displacement of the contents of the container (eg, of tablets), the outlet via which the tablets can be dispensed is preferably located at the base of the container.
Commonly, the center axis (bottom to top) of the container is vertical, but deviations of up to 45 ° are possible as long as the selected angle of deviation of the container from verticality does not significantly affect the intra-container flow of tablets from the container body to the element. distributor. In some embodiments, only part of the container can deviate from typical horizontal and vertical orientations. For example, the base of the container, or part of it, can be tilted (eg to improve flow towards the container outlet) thus deviating from horizontality, while the walls are essentially vertical.
The base, wall (s) and top of a container may form an integral part or may remain separable. Sections of the wall (s) or the top of the tablet container may be movable or removable (eg, hinged, screwed, sliding, plug-in, etc.) to allow filling of the container with tablets. This alternative is particularly appropriate when the containers are non-reversibly connected to a platform, as described later herein. Furthermore, the container may comprise sections of different transparency or levels of opacity. for example, the container can be non-transparent for most of its surface, with a transparent window above or along the walls that allows visual monitoring of the contents of the container and the level of the tablets in it. Alternatively, most parts of the containers can be transparent.
In some embodiments of the invention, one or more of the tablet containers further comprise a desiccant, which has the object of reducing the humidity of the environment within the container. In some embodiments, the desiccant is enclosed within a suitable housing. In some embodiments, the desiccant is encapsulated or bagged in any permeable material allowing its activity, as is standard in the field of desiccation.
The desiccant can be placed inside the container or be connected by any appropriate means to the top of the container and / or its walls, as long as the position of the desiccant does not affect the flow of the tablets.
Alternatively or in addition, one or more desiccants may be located in other appropriate parts of the device to reduce the extent to which the tablets are exposed to moisture, as long as the placement of the desiccant housing does not impede the flow of the tablets. A container comprising a desiccant is schematically illustrated in Figure 6.
Suitable desiccants include, but are not limited to, silica gel, calcium sulfate, calcium chloride, potassium chloride, montmorillonite clay, activated alumina, and molecular sieves (such as aluminosilicate minerals, clays, microporous carbons, zeolites, carbons activated or synthetic compounds). The containers to be used in the dispensing device may have any appropriate shape that allows free intra-container movement of the tablets. Appropriate horizontal cross sections of a container include any regular shape such as a circle, ellipse, square, rectangle, oblong, triangle, or polygon. Less regular or irregular cross sections may also be appropriate as long as they are appropriate for the selected dispensing element and compatible with the connection of containers to the dispensing means. For example, containers having an approximate triangular section with a convex face could fit like slices of a cake to together form a conglomeration of containers in roughly cylindrical shape.
Examples of individual containers according to some of the embodiments of the invention are illustrated in Figures 4-6, and multi-compartment containers are illustrated in Figure 7.
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Figures 4A-4D show non-limiting examples of containers. Figures 4A and 4B both illustrate containers having the same shape along their axis from base to top, different from each other in height. In an exemplary embodiment of the invention, the containers shown in Figures 4A and 4B have wall heights of 170mm and 320mm, respectively.
Figures 4C and 4D both show containers with different shapes along their axis from base to top, different from each other in height. In an exemplary embodiment of the invention, the containers shown in Figures 4C and 4D have wall heights of 160mm and 310mm, respectively.
The floor of the wall section of the containers illustrated in Figures 4C and 4D is sloped towards the base section and the dispenser element to ensure that essentially all of the tablets found in such containers can be dispensed.
As illustrated in Figures 7A and 7B, the multi-compartment containers 71 may have a horizontal surface area and an overall volume corresponding approximately to the sum of the horizontal area and volume of each of their individual internal containers 73. The alternative elements previously described for separate individual containers apply to the internal individual containers of a multi-compartment container, provided that the selected parameters are compatible with the fact that adjacent internal containers may share part of the internal walls. 75 that divide the overall capacity of the container into compartments.
The internal compartments, or containers 73, of a multi-compartment container 71 may be the same size, as schematically illustrated in Figure 7A. Alternatively, the individual inner containers can be of different sizes, as illustrated in Figure 7B. The internal containers of a multi-compartment container may share with each other, and optionally with all internal compartments of the same larger container, the same base and / or the same top section. As for individual containers, each inner container of a larger multi-compartment container has an outlet shown schematically in Figures 7A and 7B as a dotted circle 77. For clarity, the outlets are depicted on only part of the inner containers. The multi-compartment container may have in its upper section a lid common to all internal containers. Alternatively, each inner container may be individually sealable allowing one container to be opened at a time.
In an exemplary embodiment of the dispensing device, all the tablet containers are the same size and each contains a different type of tablets, as detailed hereinafter. However, since certain tablets may be used more frequently or may be used in larger numbers in the preparation of a coloring composition or any other composition for treating hair, the device may alternatively comprise one or more tablet containers having a larger volume. large to accommodate a larger number of such tablets. This alternative could improve convenience by having relatively similar tablet fill or cartridge replacement rates or rates. Alternatively and / or additionally, such frequently used tablets may be located in more than one container. An example of a most commonly used type of tablet is the natural base shade.
The cross-sectional geometry can also vary within the same container section. For example, the wall section may be smaller and / or differently shaped in a subsection to facilitate grasping of the container and / or viewing the contents of the container.
The surface area of the horizontal cross section of the container can vary from 1 cm<sup>2</sup> at 250 cm<sup>2</sup> or about 10 cm<sup>2</sup> about 200 cm<sup>2</sup> (and be the same or different along the axis from base to top).
The volume of a container or a single compartment within the multi-compartment container can be as desired and generally varies from 250 cm<sup>3</sup> at 5,000 cm<sup>3</sup>. Exemplary vessels have a volume of around 500 cm<sup>3</sup>, 1,000 cm<sup>3</sup>, 2,000 cm<sup>3</sup>, and 4,000 cm<sup>3</sup>, the term around meaning + 10%.
A container or compartment may contain a quantity of tablets in a range of about 100 grams to about 3,000 grams, including smaller and larger amounts, depending on the volume of the container and the shape and density of the tablets. Assuming a packing density of about 50%, exemplary containers enclose about 300 grams, about 600 grams, about 850 grams, or about 2,000 grams ± 10%.
In multi-compartment containers, the horizontal surface area and an overall volume roughly correspond to the sum of the horizontal area and volume of each of its individual internal containers. Any of the elements described for separate individual containers apply to the internal individual compartment of a multi-compartment container, as long as the selected parameters are compatible with the fact that adjacent internal containers may share part of the internal walls dividing the compartment. overall cavity of the container into compartments.
ES 2 823 977 T3
In order to facilitate the replacement of a container without the tablets spilling when they are separated from the distributor element, especially in the case when the distributor element is not located in the container, shutter means can be used which automatically closes the outlet of the container. container when the container is removed from its position.
Figures 41 and 43 illustrate two examples of such shutter means. In the example shown in Figure 43, two partial spherical covers 240 and 242 are used, held together by rubber or rubber bands 244 when the container is outside the dispenser, but is opened when the container is inserted into the dispenser.
In Figure 41, a rubber cap 24 6 perforated in its center is used, its perforation is small enough to prevent the tablets from falling out of the container. When inserted into dispenser 248, the perforation is stretched by a rigid tube 250 designed for that purpose, such that the beads can now be poured through it from the container to the dispenser member.
The distribution unit:
Each of the containers and / or compartments of the dispensing device is directly or indirectly connected to a unit to supply its contents. The device therefore comprises a dispensing unit for supplying tablets from the tablet containers. In some embodiments, the device contains a unit for delivering tablets in a predetermined quantity.
In some embodiments, the dispenser unit and the tablet container are connectable with each other.
The dispensing unit can be anything capable of accurately and measurably dispensing tablets (eg, one at a time). Appropriate means include weighing and counting the tablets.
Thus, in some embodiments, the dispensing unit comprises means for weighing or counting the tablets thereby providing a predetermined quantity of the tablets that is supplied from each of the tablet containers.
Counting can be performed with the assistance of electronic components (eg, an electronic sensor) or using a mechanical implementation (eg, spinning a sprocket, as detailed later herein). In some embodiments, more than one of the implementations described above can be combined, (for example, tablets are first counted by a mechanical system, and the number of tablets is further queried by electronic components or a combined electromechanical system is used).
Examples of electronic sensors include optical sensors, capacitive sensors, and acoustic sensors, which can be placed at any appropriate point along the path of tablet administration. When placed flush with the container outlet, each container needs to be monitored by at least one optical sensor, while acoustic sensors can monitor one or more containers. Preferably, corrective action can be taken in the case of inaccurate supply.
To improve accuracy, the dispenser unit may further comprise a spacer element 222 that prevents more than one tablet from being dispensed at a time. In the case of a sprocket, the spacer element is positioned above the section of the sprocket that overlaps the outlet of the tablet container. The spacer element prevents the tablets from immediately entering the tooth space from which a tablet was delivered while the tooth space is positioned above the outlet.
The spacer element ensures that only the tablets located in the subsequent tooth spaces are distributed, if so desired and controlled by the rotation of the tooth 220. To achieve this objective, the separating element 222 can for example be located at a height above the sprocket, allowing the passage of a single tablet (that is, slightly above the thickness of a tablet that has entered a space of tooth), but prevent the passage of two tablets stacked one on top of the other (that is, below the thickness of two tablets, one being in a tooth space). Any other placement that serves the exact supply purpose is appropriate.
While the spacer 222 is theoretically an element of the dispensing means, in practice, according to some embodiments, the spacer may form part of the container, and still be in communication with the dispensing means. In one embodiment of the invention, the spacer element is a wire, which optionally passes through beads, or a thin stem connected between two points on the internal walls of the container, said wire or stem runs over the sprocket through of the length of the container outlet. When gear 220 is located in the base portion of the container, the wire or stem can be connected to the inner walls of the base. Alternatively, the spacer element may be a rib
Plastic ES 2 823 977 T3 connected to or molded into the tablet container as part of the tablet container.
Tablets can be dispensed from containers either sequentially, one container only begins dispensing after the previous container has completed dispensing or concurrently, all relevant containers dispense at approximately the same time.
The dispenser unit may be located within the container providing controlled access of the tablets to the outlet of the container, preferably by being located above the outlet. Alternatively, the dispensing means may be located outside the container providing controlled exit of the tablets from the container outlet, preferably by being located below the outlet.
The dispenser unit can be positioned above or below a platform, as described later herein. When the distribution unit is composed of two parts and more, some part (s) can be placed above the platform and other part (s) can be placed ( s) under the platform.
An example of a distributor unit that comprises more than one part is a sprocket that has a motor that rotates the wheel in a controlled manner.
Figure 5 shows a detailed view and a cross-sectional view of an exemplary container and dispensing means. For clarity, not all parts referred to in one view are necessarily indicated in the other view.
An exemplary cylindrical tablet container 11 is shown in Figure 5, comprising container walls 31, a top 33, a container base 35, and a container outlet 55. The base container base 35 has an opening 37 that allows connecting the container to or through an optional platform (not shown herein and shown for example, as item 17 in Figures 1 and 2). The connection can be secured by means of a toggle bolt 39. The base opening of the container allows the passage of the shaft 41 of the stepper motor 43. The motor shaft 41 can be terminated by a shaft head 45.
A distributor element 13, consisting of a sprocket 47, comprises numerous teeth and tooth-spaces between adjacent teeth, as individually illustrated by tooth 49 and tooth-space 51. Sprocket 47 can be connected to the motor shaft 41 by mating the shaft head 45 through a socket of corresponding shape and size with the shaft head. Such a receptacle is placed under the sprocket on the face facing the motor, it is not shown in Figure 5. In addition to Figure 5, a separating element 53 is shown that prevents access of a new tablet to the space ( tooth s) located above the container outlet 55.
Figure 6 shows a detailed view and a cross-sectional view of alternative embodiments for the container and dispensing means. For clarity, not all parts referred to in one view are necessarily indicated in the other view. The upper part of the container 33 is shown as a plug that can be inserted into the upper portion of the container walls 31. This plug allows the insertion of a desiccant 61 into the container. In addition to the already described container base 35, the lever bolt 39, shaft head 45, sprocket 47 and spacer element 53, (see, for example, Figure 5), the device comprises an internal funnel 63. The internal funnel 63 is able to support part of the weight of the tablets, reducing the pressure on the sprocket 47, and the height of the tablets that could be distributed during the rotation of the sprocket. The inner funnel 63 can promote a long service life of the stepper motor 43 (see, Figure 5) and the distributor unit as a whole. The inner funnel 63 is preferably located closer to the base than the top of the container, the narrow section of the funnel pointing downward. The stepper motor and its shaft can be connected via the shaft head to the sprocket not shown. Alternatively, the internal funnel can be located outside the container thereof, between the container outlet and the dispenser unit (gear).
Figure 8 shows a top view of an exemplary sprocket 4 7 allowing a more detailed view. In Figure 8, the outlet of the container 55 is illustrated by a gray shape having a length of approximately 59. The circle surrounding the sprocket may be a projection of the walls or base of the container. The general position of toothed wheel 47 above the base of the container comprising the container outlet is arbitrary for purposes of illustration, since, as indicated hereinabove, the dispensing means could be positioned below the container outlet. A length 57 of a tooth-space 51 that is located between two adjacent teeth 4 9 is less than the length 59 of the outlet of the container. The length 57 of the tooth space is selected to allow the delivery of only one tablet and can be designed according to the size of the tablets to be dispensed. The length 59 of the outlet of the container 55 is selected to allow rapid delivery of the tablets, taking into account the tangential speed of a tablet being rotated by the wheel (that is, by the stepper motor), while allows the passage of only one tablet by the controlled rotation of the wheel.In general, the length 59 of the container outlet is up to
ES 2 823 977 T3 two to three times the length 57 of a tooth space and a length of a flanking tooth.
The prevention of the uncontrolled passage of the tablets through the outlet of the container 55 is also obtained by means of the separator element 53, as shown in Figure 4 as a wire that runs between two points of the container along the length of container outlet 55.
A dispensing unit (or element) can be located within the container providing controlled access of the tablets to the outlet of the container, preferably by being located above the outlet. Alternatively, the dispensing means may be located outside the container providing controlled discharge of the tablets from the container outlet, preferably by being located below the outlet.
The dispensing means can be positioned above or below a platform, as described later herein. When the distribution means are composed of two parts and more, some part (s) can be placed above the platform and other part (s) can be placed ( s) under the platform.
An example of a distributor unit that comprises more than one part is a sprocket that has a motor that rotates the wheel in a controlled manner.
Thus, in some embodiments, the dispensing unit comprises means for weighing or counting the tablets to thereby provide a predetermined quantity of tablets that is supplied from each of the tablet containers.
Reference is now made to Figure 42, which shows in greater detail one possible embodiment of the tablet dispenser 200 of Figure 40.
Figure 42 illustrates an embodiment of the tablet dispenser in which the base of the tablet container 215 (See Figure 40) contains respective dispensing mechanisms 203 based on rotating sprockets that are positioned above the platform 205 to which they are connected. , while the corresponding stepper motors 207 are placed under the platform 205. The outlet of the containers are positioned above the platform openings in such a way that the tablets are supplied to the channel 209 (see Figure 40), located below the platform 205, and from there by gravity to the outlet of the tablet 211. In this exemplary embodiment, the platform can be supported by a single leg.
As discussed in connection with prior embodiments, the number of tablets that are delivered is proportional to the extent of rotation of sprocket 22 0 as controlled by the stepper motor. This number depends on the degree of rotation, the circumference of the sprocket, the number of teeth on the wheel, the tooth-gap length and the like, all are factors that can be easily adjusted by the person skilled in the art with the in order to distribute the desired numbers of tablets. As the sprocket rotates, the tablets fall under the gravity of the tablet container body to replace the dispensed tablets, filling the sprocket tooth spaces for subsequent dispensing. For example, for a sprocket that has 24 tooth spaces and that rotates at a maximum speed of 12 0 RPM, as many as 48 tablets could be delivered per second. Even lower delivery rates of about 25 to 35 tablets per second ensure that all the tablets necessary for the preparation of a desired coloration are provided by the device according to an exemplary embodiment of the invention in a short time that does not exceed ten seconds. Such a quick process advantageously replaces long combinations of human tones.
Reference is now made to Figure 44 which is a detailed view and a cross-sectional view of an exemplary container and dispenser unit. For clarity, not all parts referred to in one view are necessarily indicated in the other view.
An exemplary cylindrical tablet container housing 511 is shown in Figure 44, comprising container housing walls 531, a platform 205, and a container outlet. The connection can be secured by means of a toggle bolt 539. The base opening of the container allows passage of the shaft 541 of the stepper motor 207. The motor shaft 541 can be terminated by a shaft head 545.
A distributor element 513, consists of a sprocket 547, comprising numerous teeth and tooth spaces between adjacent teeth, as individually illustrated by tooth 220 and tooth-space 557 in FIG. 42. The sprocket 203 can be connected to the motor shaft 541 by matching a shaft head 545 through a socket of a shape and size corresponding to the shaft head using a rubber or rubber plate 230 and clutch 232 as shown in Fig. 42. Such a receptacle which is placed under the sprocket on the face facing the motor, is shown in Fig. 42. Shown further in figure 44 and more clearly in figure 42, is a separator element 222 that prevents access of a new tablet to the space (s) of the tooth (s) located (s) above the exit of the container.
ES 2 823 977 T3
Figure 45 shows a top view of the tablet dispenser 200 of Figure 40 and shows the top of the container 580 as a cap can be inserted over the dispensers as shown in the side view in Figure 41.
Figures 3A-E show various possible combinations of containers on the platform of the dispenser device, in accordance with some exemplary embodiments of the invention. Such exemplary containers can be used in various possible combinations in the devices of the invention. Figures 3A-E present non-limiting possible combinations of containers. In Figure 3A, all the containers have the same shape and size. In Figure 3B, all the containers have various sizes. In Figures 3C, 3D and 3E, the containers differ in shape and size.
Provided that the various combinations of vessels are connected to a universal platform, the device can be designed to suit a variety of uses and end users. For example, small size containers can be used for less frequently used shades, such as blue or for a small beauty salon and large size containers for more frequently used shades or for furnishing warehouses.
Return the tablet dispenser and the outline of the sprocket may be a projection from the walls or bases of the container. The position of toothed wheel 220 above the base of the container comprising the container outlet is arbitrary for purposes of illustration since, as indicated hereinbefore, the dispensing means could be positioned below the container outlet. . A length 557 of a tooth-gap 551 located between two adjacent teeth 549 is less than the length of the container outlet. The length 557 of the tooth space is selected to allow delivery of only one tablet and may be designed according to the size of the tablets to be dispensed. The length of the container outlet is selected to allow rapid tablet delivery, taking into account the tangential speed of a tablet being rotated by the wheel (that is, by the stepper motor), thus allowing the passage of only one tablet per controlled rotation of the wheel. In general, the length of the container outlet is up to about two to three times the length 557 of a tooth gap and the length of a flanking tooth 549.
Prevention of uncontrolled passage of the tablets through the container outlet is also achieved by means of the separator element 222, an alternative of which is shown in Figure 4A-D as a wire running between two points of the container along of the length of the container outlet 55.
The platform:
As mentioned hereinbefore, in some embodiments, the dispenser unit further comprises a platform to which the containers and / or compartments are connected.
In some embodiments, the containers / compartments and the dispensing unit are connectable to each other through the platform in such a way that, for example, the containers are placed above the platform and the dispensing means are positioned below the platform.
In other embodiments, both the containers and dispensing means are positioned above the platform.
In some embodiments, each of the tablet containers and / or the dispenser unit is connectable to the platform. The connection can be non-reversible, if it is permanent or reversible, if the container can be connected to and detached from the platform more than once. Reversible connection assemblies, for example, single-use cartridges and / or allow access for maintenance. A single-use cartridge is a disposable container pre-filled with tablets of interest (basic shades or rapid disintegration media tablets).
The connection of the platform can be made by any appropriate means, for example by means of mating openings in the platform, the containers and the dispensing means. For example, the containers and platform can be connected by means of spring loaded bolts and receptacles. Alternatively or additionally, the connection may be by means of the platform between device components located above the platform (for example, the containers) and device components located below the platform (for example, if the dispensing means are thus located ). For example, the shaft of a motor could connect the motor by means of a distributor element to a corresponding container.
In some embodiments, the platform is perforated to allow through flow of tablets from their respective containers. The perforated platform may either be suitable for one type of container of given shape and dimension or may alternatively accommodate more than one type of container, hence serving as a universal platform.
The platform may be at various angles between horizontal and vertical and may comprise one or more legs than the
ES 2 823 977 T3 are supported at the desired angle in relation to a horizontal work plane or a vertical wall. The support leg (s) allow for proper positioning of the various components of the device in relation to the platform and to each other. Preferably, the containers are above the platform which in turn is in an elevated position relative to the funnel (s), tube (s) and tablet outlet (s). When the platform is vertical, the containers are above the platform by being tilted relative to the platform, such that the upper sections of the containers are in an elevated position relative to the platform allowing the tablets to flow down. under. The tablet outlets or outlets of the device are appropriately positioned for convenient excess of the receiving container (s) below them when the device is in use.
The device may further comprise a device housing that fully or partially encloses some or all of the device's components. In an alternative embodiment, the housing provides support for the platform.
As mentioned, the platform of the device according to the invention can accommodate containers of different sizes and shapes. As described, all containers can be individual separate containers. Alternatively, all of the containers may be part of one or more multi-compartment containers. In a further alternative, some of the containers are individual containers, while the other containers are part of one or more multi-compartment containers.
As long as the various container combinations are connected to a universal platform, the device can be designed to suit a variety of uses and end users. For example, small size containers for less frequently used shades, such as blue or for a small beauty salon and large size containers for more frequently used shades or for supply stores).
Additional components and operation:
In some embodiments, the device comprises, in addition to the tablet containers, the tablet dispensing means and the optional platform, additional components including for example legs that support the platform, as described hereinbefore, housings capable of enclosing the minus part of the device, as described earlier herein, one or more funnels and / or tubes to transfer the dispensed tablets to one or more tablet outlets, one or more pedestals to receive containers capable of holding the customized combination of tablets and optionally any additional means supplied from the device or in communication with it and user interfaces capable of providing or retrieving information concerning the customized combination of tablets.
Figure 1 is a detailed view of an exemplary dispenser device in accordance with some embodiments of the invention. Each of the tablet containers 11 comprises in its base portion a dispensing unit 13 composed of a rotating gear wheel and a stepper motor 15. The containers and their respective dispensing means are placed above the platform 17 at the which are connected. A funnel 19, arranged under the platform, guides via its slopes the tablets distributed to the tablet outlet 21. A receiving container (not shown in figure 1) can be placed on the base 23, below the tablet outlet 21 to collect the distributed tablets. In this exemplary embodiment, the device comprises a housing 25 that supports the platform (and parts attached thereto) and encloses the funnel. Base 23 can provide partial sealing of the housing. Figure 1 schematically illustrates how a user interface 27 can be included in the device.
Figure 2 shows alternative exemplary embodiments of the device in detailed view and perspective view. For clarity, not all parts referred to in one view are necessarily indicated in the other view. In this figure, the tablet containers 11 and their respective dispensing means 13 based on rotating sprockets are placed above the platform 17 to which they can be connected, while the corresponding stepper motors 15 are placed below the platform. . The container outlets are positioned above the platform openings such that the tablets are delivered to a funnel 19, located below the platform and hence by the gravity of the tablet outlet 21. In this exemplary embodiment, the platform is supported by a single leg 29.
Reference is now made to FIG. 40 which illustrates in detail view an overall dispenser device in accordance with the present embodiments comprising a tablet dispenser 200, a media dispenser 210, and a receiving container 212.
In some embodiments, dispenser unit 210 and tablet dispenser 200 are connectable with each other.
The dispensing unit can be anything capable of accurately and measurably dispensing tablets (eg, one at a time). Appropriate means include weighing and counting the tablets, as described herein.
ES 2 823 977 T3
Each of the tablet containers 202 is associated with respective dispensing elements 203 comprised of a rotating gear wheel and a stepper motor 207. The containers and their respective dispensing means are positioned above the platform 205 to which they can be connected. A conduit 209, located under the platform, delivers the distributed tablets via its slopes to the tablet outlet 211. A receiving container 212 may be positioned below the tablet outlet 211 to collect the dispensed tablets. In this exemplary embodiment, the device comprises 3a the housing 213 that supports the platform (and parts connected thereto) and encloses the funnel. A base can provide partial sealing of the housing.
The tablet dispenser 200 may comprise multiple containers 202 each having an approximately triangular cross section with a convex face 204, such containers fit together like slices of a cake and together form a container arrangement of approximately cylindrical shape. One or more containers can be placed in space 208 that is formed around the center of the cylindrical arrangement. The additional containers may have an approximate triangular cross section with a convex face and may also fit like slices of a cake and together form an array of inner containers approximately cylindrical in shape within a diameter that is smaller than the outer cylindrical array. Alternatively, the additional containers may have a different shape than the triangular shape, which fits the space formed around the center of the cylindrical shape.
In addition, the containers 202 and 206 can be either individual separate elements or parts of a larger container appropriately divided with one or more internal walls to form a multi-compartment element consisting of two or more individual containers.
Containers 202 and 206 can vary in geometry along the base to the upper axis. For example, the containers may have an unregulated cross section in the vicinity of the base portion (for example, capable of accommodating dispensers of appropriate geometry), other geometry in addition to the wall portion (for example, oblong, rectangular, square, etc.) and optionally still a different shape in the upper portion (eg capable of accommodating a lid).
In some embodiments, the dispensing device comprises, in addition to the tablet containers, a tablet dispensing mechanism and the optional platform as described herein and one or more funnels and / or tubes configured to funnel dispensed tablets from the tablet container. to an exit.
Thus, in some embodiments the tablets may flow under gravity or mechanically, from the container outlet directly or indirectly to one or more funnels. Indirect flow indicates that a tube of appropriate dimensions can be used intermediate the outlet of the container and a funnel. The funnel may have sloping walls that channel a freely flowing tablet out of the funnel. If more than one funnel is used, each funnel can independently channel tablets from one or more outlets of the container.
Alternatively, the tablets may be transferred from the dispensing unit to the collection container 212 in a motorized manner, for example a conveyor belt. This would generally reduce the overall dealer reading.
The tablets flow (eg, under gravity) through the funnel (s) directly or indirectly to the respective tablet outlet of each funnel. Indirect flow indicates that a tube of an appropriate dimension can be used in an intermediate position between the funnel outlet and the tablet outlet through which the appropriate amount and types of tablets are delivered to the receiving container.
In some embodiments, the device may further comprise one or more tubes connecting the outlet of the tablet to an inlet of a portion subsequently connected through the outlet of the device.
If more than one funnel and / or tube is used to transfer the tablets being delivered, the device may further comprise a converging funnel or tube that routes all tablet outlets to a single device outlet. If the device comprises a single funnel or tube, the individual tablet outlet is alternatively referred to as the device outlet.
The outlets of any element of the device may further comprise a one-way valve. The one-way valves, whether controllable or not, allow the tablet to flow out of the corresponding device element when they are in the open position, while reducing the access of eventual degradation factors when they are in the closed position.
The tablets can be channeled through the channels and / or tubes described above into a receiving container where they are mixed with an aqueous medium or mediums to provide a composition to treat the
ES 2 823 977 T3 hair (eg, a coloring composition), as described herein.
The device may comprise a weighing unit to provide further indication of the quantity of tablets being dispensed, further increasing the reliability of the dispenser.
The device may comprise a detection unit that detects the absence of a receiving container at the outlet of the device, reducing the probability that the tablets dispensed without harvesting the tablets. The detection unit can comprise for example optical, capacitive, electrical, magnetic and / or mechanical detection.
The device may comprise a replacement mechanism to facilitate replacement of a certain container (eg, when emptied), by moving the container to a specified location that is appropriate for replacement. Referring again to FIG. 45, the replacement mechanism may comprise a sprocket 590, optionally driven by a motor.
The device may comprise container recognition to reduce the probability of misplacing a certain container in an incorrect position. The recognition of the container can comprise for example optical means, RFID means and mechanical means.
In some embodiments of the invention, the device delivers the desired set of tablets to the receiving container and the media is then manually measured and added.
Alternatively, the device may further comprise one or more media containers and optionally one or more media distribution elements configured to measure the amount of media that is transferred from the media containers. In some embodiments, the device further comprises one or more funnels or tubes for transferring the distributed media to one or more media outlets. The media outlet can distribute media to the same receiving containers as the desired sets of tablets or to additional media receiving containers.
In some embodiments, the device further comprises at least one additional container that comprises an aqueous solution and is in communication with at least a portion of the compartments that comprise the at least active agent, the device is configured to generate a predetermined amount of the medium. after one type of tablets with the aqueous solution.
The principles guiding the selection of appropriate media and dispenser containers for devices according to the invention are as previously stipulated for tablet containers, with appropriate settings required to store and distribute liquids of relevant viscosity and chemical reactivity in a measurable manner. For example, the media can be distributed using piston-cylinder systems or pumps. In some embodiments, the liquid media is fed through a separate outlet from the dry tablet outlets. In some embodiments, the liquid media is delivered through the tablet outlet, for example by means of one or more funnel tubes through which the liquid media passes and flows to the one or more funnels and tubes through the which tablets pass to the output of the device.
In some embodiments, the plurality of containers comprise two or more types of tablets, contained separately, contained in such a way that a container of tablets comprises one type of tablets. The dispensing device is operated such that a certain combination of two or more tablets are dispensed, thereby providing a desired combination to form the hair treating composition. The composition would comprise a desired predetermined combination of the two or more types of tablets, each supplied from a different container.
In some embodiments, all containers contain color-imparting agents, which are supplied to provide a predetermined collection of color-imparting agents.
In some embodiments, at least one type and optionally all types of the tablets comprise fast disintegration tablets, as described herein.
In some embodiments, one or more types of the tablets comprise an oxidizing agent, an alkaline agent, and / or a thickening agent.
Such tablets can be used either per se (eg, to form a bleaching composition) or in combination with tablets comprising a color-imparting agent or any other form of color-imparting agents.
Each of the above tablets may be co-dispensed or otherwise mixed with an aqueous medium (s), which may simply be an aqueous diluent or may comprise active agents of
ES 2 823 977 T3 complement to effect the desired treatment.
Figure 46 shows in greater detail the media dispenser 210 and receiving container 212 part of Figure 40. The media dispenser 210 comprises funnel-shaped media containers 580 that also have dispenser mechanisms 582.
The media dispenser 210 may comprise a dispenser mechanism 582 for supplying the media from the media containers 580. The dispenser mechanism 582 may comprise a piston (not shown in the figure) for focusing the media out of the containers 580. It can be activated using pneumatic elements, an electric motor or electromagnetic or magnetic elements. The piston may or may not be part of the container. Alternatively, the media can be dispensed out of the container without the aid of a piston, by pneumatic means or by the action of gravity.
The media dispenser may also comprise media valves to control the supply of media, which can be connected to the media container and one-way valve (s) 584 to keep the containers pressurized at all times in the case of pneumatic operation. . A valve actuator can be used to actuate the media valves by electrical, pneumatic, or electromagnetic methods.
A single media valve and / or a single valve actuator can be used to supply media from all containers by incorporating a mechanism that brings a specific media container in close proximity to the media valve and / or valve actuator. In one embodiment, the containers can be arranged in a circular fashion and brought into close proximity to the media valve and / or valve actuator using an electric motor that rotates the container array 581 (see FIG. 45).
Media container 580 can be constructed of plastic, glass, metal, or any other suitable material. It can comprise several layers of material that allow for example: blocking atmospheric gases from penetrating the container, blocking media gases from escaping from the container, protecting the container and / or cream from chemical reaction that could occur between the container and the media, block UV light, prevent media from remaining on the inside of the container. In addition, the interior of the media container may be coated with oil, preferably thick oil to facilitate the delivery action of the media and to allow free flow of the media into the media container without the media remaining on the interior of the media. container.
The media dispenser may also comprise a prevention mechanism to prevent its operation in the event that a replaceable container has not been properly placed in position by the user, thus preventing malfunction of the device.
The media container 580 may comprise an integrated aerosol mechanism known in the art or any other integrated delivery mechanism for supplying the media from the container.
Media canisters can be replaceable or fixed. If replaceable containers are used, container recognition means can be used to reduce the probability of misplacing a certain container in the wrong position. Container recognition can comprise for example optical means, RFID means and mechanical means.
The media valve (s) can be any type of valve known in the art, appropriate for the media in use. Preferably the valve may be an aerosol valve, for example a high feed valve suitable for thick materials.
The device may also comprise a weighing unit to further improve the accuracy of the dispensed media dosing. Such a unit can allow real-time closed-loop control of the dispensed media dosage.
The device may also comprise an input / output apparatus known in the art for operating the device, such as a keyboard, mouse, screen, touch screen, and printer.
The media dispenser may comprise a way to separate the remnants of media that remain on the media valve. Such means may comprise a way to generate an air jet (s) around the media valve, for example two counteracting air nozzles connected to a pneumatic system. An alternative comprises an airtight wire that is positioned in such a way to remove the media and remains by moving the wire in close proximity to the media valve.
The media dispenser may comprise a pneumatic system to drive the delivery mechanism. The pneumatic system may comprise a pump, a compressor, electrically controlled air valve (s), one-way air valve (s) (non-return), air reservoir (s), hose (s) air and pressure gauge (s).
ES 2 823 977 T3
The media dispenser and tablet dispenser can be arranged one on top of the other, side by side or in any other suitable urine. They can be rigidly connected, loosely connected or totally separated. They may share a receiving container in an identical physical position, share a receiving container in a different physical position, or not share a receiving container.
The desired media and set of tablets may be manually mixed or the device may further comprise mixing means that are capable of mechanically mixing the desired set of tablets with automatically or manually dispensed media. Mixing can be effected by rotating an impeller within the receiving container containing the tablets and media, by applying vibrations or oscillatory movements to the receiving container containing the formula to be mixed, or by any other appropriate mixing method.
The mixing unit may comprise a driver unit, which drives a submerged driver into the coloring mixture. Alternatively, the drive unit can drive the receiving container containing the coloring mixture. The drive unit may comprise an electric motor, a magnet or an electromagnet. The use of an electromagnet allows a mixing action without direct contact of the impeller unit with the impeller and / or the receiving vessel, thus simplifying the mixing unit.
The drive unit may comprise a unit for driving a rotational movement in which the drive and / or the receiving container rotates around its center. It may also comprise a unit for driving a circular motion, in which the impeller and / or the receiving container rotates around the center of the receiving container or any other center. It may also comprise a unit for driving linear movement, for example vertical, of the impeller and / or receiving container.
The mixing unit may also comprise a unit for breaking or grinding the tablets before or after being combined with the media, if this is required.
The impeller can be specifically designed to obtain the required mixing action. Various types of impellers can be used depending on the specific coloring mix that is prepared. For example, the driver may comprise the application tool used to apply the coloring mixture to the hair (eg, brush). The receiving container can be designed to accommodate the containers currently used today in manual preparation of the coloring mixture.
Optionally, a device according to various embodiments of the invention may further comprise heating elements capable of heating the tablets and / or the media to temperatures that can increase the rate of disintegration of the tablets within the media, thus reducing mixing time. .
Optionally, a device according to various embodiments of the invention can dispense tablets while reducing or preventing premature exposure to degradation factors including for example humidity, oxygen and UV light.
The device and its parts can be manufactured from any material customary and appropriate for its intended purpose. For example, they can be made of any suitable material such as glass, metals and alloys, for example aluminum, copper, iron and stainless steel and plastic polymers, for example halogen-containing polymers, for example Polytetrafluoroethylene (PTFE), for example TefIon ®, polyacrylates such as polymethyl methacrylate (PMMA), for example Perspex®, polyoxyalkylenes, such as polyoxymethylene (POM) for example Delrine®, polycarbonates (PC), polyethylenes (PE), polypropylenes (PP), polystyrenes (PS), polyurethanes (PU), polyvinyl chlorides (PVC) and combinations thereof.
The parts of the device that contain the tablets or by means of which they are delivered (eg, containers, connecting parts, tubes, funnels, outlets, etc.) may further comprise an oxygen barrier. Appropriate oxygen protection can be obtained by using materials with low or no oxygen permeability for the fabrication of these parts. For example, metal and glass in general have low gas permeability. For plastic polymers, their crystallinity, density, level of polymerization and copolymerization, and molecular weight can affect their gas permeability and those parameters can be selected to obtain reduced oxygen permeability. Alternatively or additionally, materials that can be similarly selected to have low a no permeability to moisture or any other desired permeability or lack thereof to a factor of interest.
Alternatively and furthermore, the parts of the device involved in the containment and administration of the tablets can be connected to each other in an airtight manner and the containers and / or tubes and / or funnels and / outlets (tablet and / or device) can be , for example sealed by a one-way valve that opens, optionally controllable, only during actual delivery of the tablets. Suitable one-way valves include for example a flapper, a check valve and a relief valve (usually a lever-like ball seal located on the relevant outlet when in position.
ES 2 823 977 T3 closed). Furthermore, the connections between all or some of said parts can be externally fastened with a sealing agent. Optionally, the outlet of the receiving container device may comprise couplings that allow air-tight connection and delivery of tablets.
In another embodiment, the containers and parts of the device involved in administering tablets are protected from exposure to light (for example, enclosed in a housing or made of UV-blocking or shaded or opaque materials) or further comprise an a-blocker. UV light. Many of the plastic polymers listed above have grades that address this issue. For example Perspex® VA and grade VE block more than 99% of all UV radiation.
Furthermore, one or more of the protections mentioned above can be combined. For example, a container (and the relevant parts of the device through which tablets are administered) can be made of a non-oxygen permeable material with reduced moisture permeability which comprises a UV light blocker and further comprises a desiccant inside your body.
The device may further comprise one or more computerized systems that include a user interface that allows the input of parameters pertinent to the preparation of personalized staining formulas, databases or algorithms to determine the type and number of tablets including basic shades necessary to obtain the desired coloration and systems that provide automation of the delivery of tablets and / or media from each appropriate container. Parameters relevant to the preparation of personalized coloring formulas include, for example, information concerning the initial color of the fibers to be colored, the desired final color, individual properties of the fibers, the concentration of the color-imparting agents according to the tone tablet. basic, the strength of the appropriate media or corresponding rapid disintegration media tablets and the like. In the case of human hair, for example, the individual properties of the hair that may be of relevance, including the type of hair (for example, European, Asian, African, etc.), the texture of the hair in general (for example, straight, wavy, curved, kinky, etc.) of the individual fibers (for example, thin, thick, etc.) if the hair is not artificially colored (natural) or already partially or fully colored and other parameters such as dry types, normal or greasy and the fact that the hair can be damaged.Additional information of relevance refers to the amount of coloring formula to be prepared and this amount may vary from one individual subject to another. For example, a lower amount of formula is needed for short hair than for long hair or for coloring human hair than for coloring larger areas of non-human hair (eg, animal hair or wool).
An additional option is to have a pH tester that probes the coloring mixture after it is prepared in the container, to further increase the reliability of the dispenser (for example, not to allow overdosing of alkaline and / or oxidizing agents).
An additional option is for the hair reader system or other spectrophotometric device to measure the coloring mixture after it is prepared in the container to further increase the reliability of the dispenser (for example, not to allow misdosing of certain coloring tablets).
The determination of the types and number of basic tone tablets necessary to obtain the desired coloration can be carried out by converting the initial and final colors of the fibers to be colored to a presentation of color coordinates (for example, based on their respective spectrum. reflectance). Color coordinate displays include CIELAB, CIELUV, CIExY, CIEXYZ, CMY, CMYK, HLS, HSI, HSV, HVC, LAb, LCC, NCS, YCC photo, RGB, Y'CbCr, Y'IQ, Y'PbPr and Y 'UV. The CIELAB system, also called the Lab system, is commonly used in hair coloring, but any other color coordinates that exist or can be developed for this purpose may be appropriate. Knowing the positive or negative contribution of a tablet of each basic tone to the presentation of color coordinates, whether this contribution is linear or non-linear, one can calculate the expected change in color from the initial color coordinates to a presentation of intermediate coordinates. This step is repeated for a tablet of the same or different basic shade until the difference between the intermediate calculated color coordinate display and the desired color coordinate display is minimized. In other words, the last stage of the calculation process is reached when the delta-E number (dE) that represents the distance between the calculated and desired colors is minimal. A delta-E of 5 or less is believed to be tolerable, a delta-E of less than 1 is generally considered unremarkable to the human eye. If the coloring involves the use of oxidizing or bleaching agents or media, the initial color coordinates of an individual subject will be corrected to take into account the loss of natural pigmentation, if any. Alkaline agents and thickening agents can affect the penetration of the fibers and the effectiveness of the lightening or coloring. Preferably, the contribution of each active agent when present in the final coloring formula is taken into account in the calculations mentioned above. This method can provide the number and combination of basic shades to be distributed to obtain the desired set of tablets.
Assignment of color coordinates to the start and end colors can be done manually by visual selection from appropriate databases or catalogs of the known color coordinates of the closest possible color. Alternatively, the assignment of color coordinates to the start and end colors can be
ES 2 823 977 T3 do automatically. For this purpose, the device may further comprise a color measurement system, alternatively referred to as a hair reader system. Advantageously, the hair reader system can also take into account the individual properties of the fibers to be colored. For example, individuals who have thinner hair or a lighter initial shade may require lower amounts of color-imparting agents than individuals who have thicker hair or a darker initial shade. The optional ability to take into account the individual properties of the fibers to be colored further increases the probability of obtaining a desirable color result.
Alternatively or additionally, the hair reader system can measure the spectral reflectance of the hair to be colored, further increasing the probability of obtaining a desirable color result. The spectral range could be 200 nm to 1,300 nm, preferably 300 nm to 1,100 nm, preferably 380 nm to 970 nm. The measurement resolution could be 1 nm to 200 nm, preferably 2 nm to 10 nm, preferably 4 nm.
The device may further comprise a computerized system that allows tracking the amount of tablets and / or media consumed from the connection of the cartridge or filling of the containers. Such a monitoring system can trigger an alert when the remaining quantity of tablets of a given type reaches a critical level that requires inventory availability for replacement or refilling. The critical level can be set individually for each type of tablet (for example, 10 times the average number of tablets of a basic shade in the coloring formula) or it can be set uniformly for all tablets (for example, about 100 tablets. or 500 tablets, etc.).
The device may further comprise memory and / or connectivity means for storing and / or transferring desirable information. For example, the device can store for future use information concerning the set of tablets that provide a desired coloring formula to a specific consumer. Such information can be stored independently in each beauty salon or retail store served by a consumer or centrally in an external Pluggable database of each device independent of location. Such connectivity of independent sites to information relevant to specific consumers can further improve the reproducibility of the coloring formula or increase the probability of obtaining a desirable color result should a hair color change be desired by the customer. The device may also comprise a hatch that allows storage of desirable information to a portable memory system (eg, a consumer USB key or slide card).
The connectivity of the device's computerized systems can be to Connectable units internal to the beauty salon or retail store and external units to those locations. For example, the system that tracks the number of consumed / remaining tablets can be connected to an internal purchasing system to trigger an alert and / or to a new inventory provider to directly connect an order. Such connectivity (eg via a receiver-transmitter) can serve any other desired purpose, eg for billing purposes.
The device according to the invention can also comprise at least one printed circuit board (PCB) to mechanically support and electrically connect the electronic components of the device and any conventional parts (eg Connectivity to the power grid, etc.).
In some embodiments, the device as described herein is connected to a computational unit as described in greater detail earlier herein.
In some embodiments, the device is connected to an optical reader as described in greater detail earlier herein.
Selecting a tablet combination:
In the following, reference to tablets also includes concentrations of oxidizing and alkaline agents, bleaching, treatment time and other color treatment parameters also as tablet combination.
In any of the methods and devices described herein, the selection of a tablet combination can generally be accomplished by: establishing the initial color and condition of the hair (eg, hair), fibers, and then selecting a desired custom color or other treatment that is tailored to an individual subject. The custom treatment could be selected by the user from a collection of final shades as desired. The system is then in position to determine appropriate tablet amounts, in combination, to treat the fibers as desired by the customer.
Establishing such an initial color may involve measuring an initial reflectance spectrum. The custom color selection may comprise determining a reflectance spectrum of the custom color and the reflectance spectra may be independently converted to a display of color coordinates.
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The amount of tablet to be used can be determined by adding to the initial reflectance spectrum the positive or negative contribution of a tablet of a basic shade to obtain an intermediate calculated color coordinate display. Then, iterations of the calculation step can be carried out for a tablet of the same or different basic shade until the difference between the intermediate calculated color and the desired color coordinate display is minimized.
The determination can take into account positive and / or negative contributions of an active agent such as an alkaline agent, an oxidizing agent or a thickening agent to the calculated color coordinate display.
The selection can take into account the contribution of individual properties of the hair.
The selection can be carried out by a computer implemented system.
The measurement can be carried out by the optical hair measuring device or hair reader. The hair reader may comprise an illumination unit for removing hair and a measuring unit comprising at least one sensor for optically measuring hair during illumination. The sensor and a beam of the lighting unit can respectively subtend a light scattering angle in the hair that is measured, thereby ensuring that the sensor mainly measures the light that is scattered or scattered by the hair.
The hair reader may include a main light source and subsidiary light sources and processing electronics to use differential lighting results from the various sources to determine the angle of the hair in relation to the main light source.
The main light source can be used for spectroscopy and a subsidiary light source can be used for angle measurement.
The sensor comprises sensitivity to the visible and near infrared parts of the electromagnetic spectrum.
Reference is now made to Figure 47 which is a simplified diagram illustrating an embodiment in which a hair reader provides inputs for color prediction and color prediction in turn controls the dispenser to supply the dye that is necessary for get the desired color.
In FIG. 47, the hair reader 600 reads the hair, with particular attention to specular reflection and light scattering as explained as these provide extensive information regarding the condition of the hair. Additional information is obtained beyond the visible spectrum, as explained above.
The user requests a particular end result, a desired hair color via user input 602.
The color prediction system 604 now has a user request and detailed information regarding the condition of the user's hair at a variety of wavelengths. The color prediction system is now able to predict the resulting color if different dye mixtures were applied to the wearer's hair, using the methodology previously described herein.
Once a mixture of dyes is found whose prediction indicates the color required by the user, then the color prediction module issues instructions to the dispenser 606 to supply the tablets and media necessary to prepare the dye.
V. Hair treatment methods:
In accordance with another aspect of embodiments of the invention, there is provided a method of treating hair, as defined herein. In some embodiments, the method is performed by disintegrating at least one tablet comprising at least one active agent (eg, a tablet described herein) in an aqueous medium (eg, an aqueous medium described herein) to thereby obtaining a composition comprising at least one color-imparting agent and contacting the composition with the hair for an appropriate period of time to provide a desired coloration.
In some embodiments, the method comprises contacting the fibers with a bleaching medium for a period of time sufficient to lighten the color of the fibers. In some embodiments, contact with the bleaching medium is effected prior to contact of the coloring composition with the fibers, for example in order to reduce or eliminate an initial color (eg, natural pigmentation) that can interfere with a color. desired imparted by the coloring composition.
The bleaching medium may optionally comprise a bleaching agent described herein.
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In some embodiments, the bleaching medium is prepared by breaking up at least one tablet comprising a bleaching agent (eg, a tablet described herein) in an aqueous medium (eg, an aqueous medium described herein). .
In some embodiments, the method further comprises mixing the tablet (s) comprising color-imparting agent (s) with at least one active agent selected from the group consisting of an alkaline agent, an oxidizing agent, and a thickening agent, for example, how such active agents are described herein. Such mixing may be before, during and / or after disintegration of the tablet comprising the color-imparting agent.
In some embodiments, mixing with at least one alkaline agent is accomplished by disintegrating at least one tablet comprising the alkalizing agent (s) (for example, a tablet described herein) in an aqueous medium ( for example, a means described herein). In some embodiments, the aqueous medium is the same medium in which the tablet (s) comprising the color-imparting agent is (are) disintegrated.
In some embodiments, mixing with at least one oxidizing agent is accomplished by disintegrating at least one tablet comprising the oxidizing agent (s) (for example, a tablet described herein) in an aqueous medium ( for example, a means described herein). In some embodiments, the aqueous medium is the same medium in which the tablet (s) comprising the color-imparting agent is (are) disintegrated.
In some embodiments, mixing with at least one thickening agent is accomplished by disintegrating at least one tablet comprising the thickening agent (s) (for example, a tablet described herein) in an aqueous medium ( for example, a means described herein). In some embodiments, the aqueous medium is the same medium in which the tablet (s) comprising the color-imparting agent is (are) disintegrated.
In some embodiments, the tablet (s) comprising the color-imparting agent is (are) mixed with an alkalizing medium comprising at least one alkaline agent and an appropriate carrier (e.g., an aqueous medium described in the present document). The alkalizing medium can optionally be prepared by breaking up at least one tablet, as described herein. In some embodiments, the concentration of the alkalizing agent (s) in the alkalizing medium is in a range of 0.1 to 15% by weight. In some embodiments, the alkalizing medium is essentially the medium in which the tablet (s) comprising (s) color-imparting agent is (are) disintegrated.
In some embodiments, the tablet (s) comprising the color-imparting agent is (are) mixed with an oxidizing medium comprising at least one oxidizing agent and an appropriate carrier (e.g., a aqueous medium described herein). The oxidizing medium can optionally be prepared by breaking up at least one tablet, as described herein. In some embodiments, the concentration of the oxidizing agent (s) in the oxidizing medium is in a range of 0.5 to 25% by weight. In some embodiments, the oxidizing medium is essentially the medium in which the tablet (s) comprising color-imparting agent (s) is (are) disintegrated.
In some embodiments, the oxidizing medium is a commercially available hydrogen peroxide solution, for example 3%, 6%, 9%, 12%, and 24% hydrogen peroxide solutions are commercially available and may be appropriate for use as the medium. oxidant according to embodiments of the invention. In some embodiments, the oxidizing medium is obtained by diluting a commercially available hydrogen peroxide solution (eg, a 24% solution) mentioned above to a desired concentration, using an appropriate amount of carrier medium (eg, water).
In some embodiments, the tablet (s) comprising color-imparting agent (s) is (are) mixed with a thickening medium comprising at least one thickening agent and an appropriate carrier (an aqueous medium described in This document). The thickening medium can optionally be prepared by breaking up at least one tablet as described herein. In some embodiments, the thickening medium is essentially the medium in which the tablet (s) comprising (s) color-imparting agent is (are) disintegrated.
Mixing of the tablets with appropriate means, as described herein can be accomplished by any technique known in the art of color mixing. If the mixing is carried out manually, the process can be carried out, for example, with a spatula, a brush, a spoon or any other appropriate tool. If mixing is done mechanically, such mixing can be done, for example by rotating an impeller within the medium to be mixed, by applying vibrations or oscillatory movements to a receiving container containing the composition to be mixed, or by any other appropriate method. .
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In some embodiments, the final coloring composition is mixed to an appropriate homogeneity for application to fibers within 10 minutes of adding the tablets to the appropriate medium. In some embodiments, the final coloring composition is mixed to an appropriate homogeneity for application to fibers for 5 minutes from the addition of the tablets to the appropriate medium.
In some embodiments, the tablet (s) comprising color-imparting agent (s) is (are) mixed with at least one oxidizing agent (eg, as described herein) and mixing The resulting product is then mixed with at least one alkaline agent (eg, as described herein).
In some embodiments, the tablet (s) comprising color-imparting agent (s) is (are) mixed with at least one alkaline agent (eg, as described herein). In some embodiments, the resulting mixture comprising an alkaline agent is then mixed with at least one oxidizing agent (eg, as described herein), to obtain a coloring composition comprising an alkaline agent and an oxidizing agent. In some embodiments, the resulting mixture is then used (eg, by mixing with an appropriate method) to prepare a coloring composition without an oxidizing agent (eg, for coloring without an oxidation dye).
In some embodiments, the tablet (s) comprising color-imparting agent (s) is (are) simultaneously mixed with at least one oxidizing agent and at least one alkaline agent. For example, the tablet (s) comprising (s) color-imparting agent (s) may optionally be mixed with an oxidizing medium that is both an oxidizing medium (eg, as described herein document) as an alkalizing medium.
For convenience, in some embodiments, where an alkalizing medium and an oxidizing medium are used, the concentration of the alkaline agent and oxidizing agent in their respective media is such that one volume of oxidizing medium is appropriate for use with one volume of medium. alkalizing.
Similarly, in some embodiments, where an alkalizing medium is used without an oxidizing medium (for example, when an oxidizing agent is used), the concentration of the alkaline agent in the alkalizing medium is such that no carrier medium needs to be added with the in order to obtain the desired concentration of alkaline agent in a coloring composition or alternatively, in such a way that the desired concentration is obtained by adding a volume of carrier medium to a volume of alkalizing medium.
It will be understood that additional volume ratios can be used (eg, one volume of alkalizing medium to two volumes of oxidizing medium if high bleaching is needed), as long as the concentrations of the active agents in the media are adjusted accordingly.
In some embodiments, the thickening agent (s) is (are) mixed with the other ingredients of the composition after all other active agents have been mixed. In some embodiments, the thickening agent (s) is (are) concurrently mixed with at least some other active agents, but no active agent is mixed after the thickening agent (s). (s) have been added. Such sequences can be useful to avoid interference from excess viscosity of mixing the ingredients.
In some embodiments, the thickening agent (s) exhibit a substantial thickening effect only after being activated by appropriate conditions. For example, some thickening agents exhibit a substantial thickening effect only at an appropriate pH. A thickening effect of such agents can therefore be activated by adjusting the pH to an appropriate pH.
In some embodiments, the thickening agent is pH sensitive and the thickening effect thereof is triggered by adding alkalizing agent (s) as described herein to a relatively non-viscous composition comprising the thickening agent, for example by adding an alkalizing medium (for example, as described herein) and / or by adding one or more tablets comprising the alkalizing agent (s) (for example, as described herein). The addition of the alkaline agent results in a relatively viscous composition.
In some embodiments, the thickening effect of the thickening agent (s) is activated after all other active agents have been mixed. In some embodiments, the thickening effect of the thickening agent (s) is activated concurrently with at least one other active agent, but no active agent is mixed after the thickening effect of the thickening agent (s). (s) has been activated. Such activation timing can be useful to avoid interference from excess viscosity in mixing the ingredients.
Thus, in some embodiments, where the activation is effected by the alkalizing agent (s), the alkalizing agent (s) is (are) mixed with the other ingredients. of the composition after all other active agents have been mixed and / or concurrently with at least some other active agents, but no active agent is mixed after the alkalizing agent (s) have been aggregate (s).
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In some embodiments, a relatively non-viscous composition comprising the thickening agent (s) (for example, prior to activation) is sufficiently acidic such that the thickening agent (s) ) does not exhibit a substantial thickening effect. Such a composition may be in the form of a medium (eg, oxidizing medium) as described herein. In some embodiments, sufficiently acidic is a pH less than 6. In some embodiments, sufficiently acidic is a pH less than 5. In some embodiments, sufficiently acidic is a pH less than 4. In some embodiments, sufficiently acidic is a pH less than 3.
In some embodiments, the tablet (s) comprising the color-imparting agent is (are) mixed with (eg, disaggregated in) an oxidizing medium comprising at least one agent. oxidant, at least one thickener and at least one appropriate carrier (eg, an aqueous medium described herein), to obtain a mixture comprising the color imparting agent, oxidizing agent and thickening agent. The oxidizing medium can optionally be prepared by disintegrating at least one tablet comprising an oxidizing agent and / or at least one tablet comprising a thickening agent, as described herein. In some embodiments, the thickening agent in the form of a powder and / or suspension (eg, aqueous suspension, non-aqueous suspension) is added to an oxidizing medium as described herein.
In some embodiments, the oxidizing medium is sufficiently acidic (eg, as described herein) such that the thickening agent (s) do not exhibit a substantial thickening effect. In some embodiments, the mixture comprising the color imparting agent, oxidizing agent, and thickening agent remains sufficiently acidic (eg, as described herein) such that the thickening agent (s) it does not exhibit a substantial thickening effect.
In some such embodiments, the alkalizing agent (s) is (are) mixed with the aforementioned mixture comprising the other active agents and a thick coloring composition is obtained with a pH, texture and appropriate viscosity (eg, as described herein). In some embodiments, the addition of the alkalizing agent (s) is accomplished by adding an alkalizing medium (eg, as described herein) to the mixture. In exemplary embodiments, the alkalizing medium has a pourable consistency (eg, a lotion, a pourable cream).
In exemplary embodiments, the active agent concentrations in the alkaline and oxidizing media are selected such that the alkalizing media and oxidizing media with the thickening agent are provided in a 1: 1 volume ratio.
In some embodiments, the concentration of the thickening agent (s) in the oxidizing medium is in a range of 0.1 to 10 percent by weight. In some embodiments, the concentration of the thickening agent (s) in the oxidizing medium is in a range of 0.2 to 7 percent by weight. In some embodiments, the concentration of the thickening agent (s) in the oxidizing medium is in a range of 0.2 to 5 percent by weight.
Examples of suitable thickening agents for inclusion in an oxidizing medium include, without limitation, acrylate polymers and copolymers thereof, acrylate-derived polymers and polymers thereof, polyvinyl pyrrolidone and copolymers thereof and polyvinyl pyrrolidone derivatives, and copolymers of same. Derivative are encompassed polymers in which at least a portion of the acrylate or PVP backbone units are substituted by one or more substituents.
In some embodiments, the concentration of the alkaline agent in the composition comprising at least one color-imparting agent (eg, after mixing) is 10 percent by weight or less.
In some embodiments, where the alkaline agent comprises ammonia, the concentration of the alkaline agent in the composition is in a range of 0.5 to 5 percent by weight. In some such embodiments, the concentration is in a range of 1 to 3% by weight.
In some embodiments, the amount of alkaline agent is selected such that the pH of the final coloring composition is in a range of 7.0 to 11.5. In some embodiments, the pH is in a range of 7.5 to 10.0.
The concentration of alkaline agent in the coloring composition and the pH thereof can affect the permanence of the coloring obtained with the composition.
In some embodiments, the amount of alkaline agent is selected such that the pH of the final coloring composition is in a range of 7.0 to 8.0, the coloring composition is for temporary coloring.
In some embodiments, the amount of alkaline agent is selected such that the pH of the final coloring composition is in a range of 8.0 to 9.0, the coloring composition is for semi-permanent and / or demi-permanent coloring.
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In some embodiments, the amount of alkaline agent is selected such that the pH of the final coloring composition is greater than 9.0, the coloring composition is for permanent coloring.
Since the pH of the composition can change after application of the composition to the fibers, the pH values described herein refer to the pH of the composition prior to application.
In some embodiments, the concentration of the oxidizing agent in the composition comprising at least one color-imparting agent (eg, after mixing) is 10 percent by weight or less.
In some embodiments where the oxidizing agent is hydrogen peroxide, the concentration of the oxidizing agent in the composition is in a range of 1 to 6 percent by weight.
The concentration of the oxidizing agent (s) in the coloring composition can be selected to be appropriate for a desired type of coloring. In some embodiments, no oxidizing agent is used in the temporary coloring composition.
Furthermore, the concentration of the oxidizing agent (s) may depend on the initial color and the desired color. For example, lower concentrations can be used when coloring a light colored fiber with a darker color than when coloring a dark colored fiber with a light color. In some embodiments, no oxidizing agent is used when coloring a light-colored fiber with a dark color (for example, when the color-imparting agent (s) is (are) not a oxidation dye).
In some embodiments, the alkaline agent concentration if the concentration of the oxidizing agent in the composition comprising at least one color-imparting agent are each 10 percent by weight or less.
In some embodiments, the ingredients are mixed and the amounts thereof are selected such that the obtained coloring composition is characterized by an appropriate viscosity to provide sufficient contact time between the composition and the fibers, thereby facilitating coloring. .
An appropriate viscosity of a coloring composition can be obtained by selecting an appropriate amount of thickening agent (if present), an appropriate ratio of liquid medium to solid ingredients, and / or an appropriate viscosity of one or more mediums used to prepare the composition. .
An appropriate viscosity may depend on the type of coloration that is intended. For example, a composition for temporary coloring may be characterized by a low viscosity (for example, a composition in the form of a wash), while effective permanent coloring commonly requires a higher viscosity such that the composition will remain in contact with fibers for a longer period of time.
In some embodiments, the final coloring composition has a viscosity of at least 50 poises or at least 60 poises (as measured at a shear rate of 10 s<sup>-1</sup>, a temperature of 25 ° C).
In some embodiments, the temporary coloring composition has a viscosity of up to 1 poise (as measured at a shear rate of 10 to about 25 ° C).
The different media used to prepare the composition (eg, alkalizing, oxidizing, and / or carrier media) may each optionally have viscosities similar to those of the final composition. Alternatively, each medium can have a different viscosity, as long as the media remains mixable and the viscosity of the final coloring composition is appropriate. In some embodiments, an alkalizing medium is more viscous than an oxidizing medium.
In some embodiments, the means comprises disintegrating at least two tablets (eg, tablets described herein), optionally at least three, optionally at least four, optionally at least five, optionally at least 10, optionally at least 20, optionally at least 50, optionally at least 100, optionally at least 150 and optionally at least 200 tablets.
In some embodiments, the method comprises disintegrating no more than 150 tablets to thereby obtain the desired color-imparting agent (s). In some embodiments, the method comprises disintegrating no more than 100 tablets to thereby obtain the desired color-imparting agent (s).
In some embodiments, the method comprises disintegrating no more than 15 0 tablets to thereby obtain all of the desired active agents described herein (ie, color-imparting agents, oxidizing agents, thickening agents, and / or alkaline agents). In some embodiments, the method comprises disintegrating no more than 100 tablets to thereby obtain all of the desired active agents described herein.
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A medium used to prepare a composition (eg, an alkalizing medium, oxidizing medium, and / or carrier medium described herein) may optionally further comprise additional ingredients, eg, an anti-dandruff agent, an anti-foam agent, antioxidants, a chelating agent. , a conditioning agent, an emollient, an emulsifying agent, a sinking agent, a free radical scavenger, a hair care agent, a humectant, an odor masking agent, an opacifier, an iridescent agent, a pH adjusting agent, a preservative, a stabilizing agent, a surfactant, a vitamin, a vitamin precursor, and a wetting agent (for example, as described herein document).
The coloring composition prepared as described herein can optionally be applied to the hair by any conventional method, for example by using a brush, a comb, a cloth, a sponge, a squeeze bottle or an applicator, including applicators that they comprise reservoirs for the coloring formula.
In some embodiments, the coloring composition is left on the hair for about 5 to 60 minutes, although certain types of memory coloring could be obtained in a shorter time.
It will be appreciated that the time for which a coloring composition must be left on the fibers is temperature dependent, which affects the speed of the coloring process. In some embodiments, coloring can be carried out at a temperature in a range of 15 ° C or 45 ° C. In some embodiments, the human hair coloring process takes about 10 to 45 minutes at room temperature.
The selection of a tablet can be based on:
set the initial color of the hair fibers and then select a desired custom color that is tailored to an individual subject. The custom color could be selected by the user from a collection of final shades. The system is then in position to determine appropriate tablet amounts, in combination, to change the color of the fibers to the customer's desired color.
Establishing the initial color may involve measuring an initial reflectance spectrum. The selection of the custom color may comprise determining the reflectance spectrum of the custom color and the reflectance spectra may be independently converted to a selection of color coordinates.
The amount of tablet to be used can be determined by adding to the initial reflectance spectrum the positive or negative contribution of a tablet of a basic shade to obtain an intermediate calculated color coordinate display. Then, iterations of the computational step can be carried out for a different base hue or tablet until the difference between the intermediate computed color and the desired color coordinate display is minimized.
The determination can take into account positive and / or negative contributions of an active agent such as an alkaline agent, an oxidizing agent or a thickening agent to the calculated color coordinate display.
The selection can take into account a contribution of individual properties of the hair.
The selection can be carried out by a computer implemented system.
The measurement can be carried out by the optical hair measuring device or hair reader. The hair reader may comprise an illumination unit for illuminating the hair and a measuring unit comprising at least one sensor for optically measuring the hair during illumination. The sensor and a beam of the lighting unit can respectively subtend a light scattering angle in the hair that is measured, to thereby ensure that the sensor mainly measures light that is scattered or scattered by the hair.
The hair reader can include a main light source and subsidiary light sources and processing electronics to use differential lighting results from the various sources to determine the angle of the hair in relation to the main light source.
The main light source can be used for spectroscopy and a subsidiary light source can be used for angle measurement.
The sensor may comprise sensitivity to the visible and near infrared portions of the electromagnetic spectrum.
In some embodiments, the measurement of an initial reflectance spectrum is performed while using an optical reader as disclosed in detail herein. However, any other hair readers are also contemplated.
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According to some embodiments of the present invention, a method of effecting a personalized hair treatment is carried out by:
obtain optical measurements of hair;
predicting the result of treating the hair with a predetermined combination of active agents and selecting, based on the prediction, a personalized combination of the active agents to effect a desired treatment of the hair and / or customized condition to apply the active agents;
preparing a composition comprising the customized composition of the active agents and contacting the hair with the composition.
In some embodiments, obtaining the optical measurements is performed using an optical reader as described herein. However, any other optical readers are contemplated.
In some embodiments, the prediction is according to the methods as described herein.
In some embodiments, at least one of the active agents is formulated as a tablet (a solid formulation as described herein) and the selection of the combination comprises selecting a combination of the tablets. Selection of the combination may further comprise selecting an appropriate medium to be mixed with the tablets to provide a desired composition, as described herein.
In accordance with some embodiments, composition preparation is accomplished by dispensing the combination of tablets from a dispensing device, as described herein.
According to some embodiments, the distributor device is interconnected with the computer-implemented unit.
In accordance with some embodiments of the present invention, the dispensing device is as described herein.
In any of these embodiments, the active agents include color-imparting agents, thickening agents, oxidizing agents, and / or alkaline agents as described herein.
In any of the above aspects, the selection is in addition to conditions for contacting the composition with the hair, where the conditions include, but are not limited to, speed, duration and temperature as described herein.
In accordance with some embodiments, any of the methods described herein are performed as long as any of the systems as described herein are used.
It will be appreciated that certain elements of the invention that are described for clarity in the context of separate embodiments may also be provided in combination in a single embodiment. Conversely, various elements of the invention that are described for brevity in the context of a single embodiment may also be provided separately or in any appropriate sub-combination or as appropriate in any other described embodiment of the invention. Certain elements described in the context of various embodiments will not be considered essential elements of those embodiments, unless the embodiment is inoperative without those elements.
Various embodiments and aspects of the present invention as outlined hereinbefore and as claimed in the claims section below find experimental support in the following examples.
Examples
Reference is now made to the following examples which together with the above descriptions illustrate some embodiments of the invention in a non-limiting manner.
Certain trademarks referenced in this document may be legal or registered trademarks of third parties. The use of these marks is by way of example and shall not be construed as descriptive or limiting the scope of this invention to material only associated with such marks.
EXAMPLE 1
Tablet compositions
Materials and methods:
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Tablets were formulated to provide a range of basic shades that can be combined to provide a customized coloring composition.
Ingredients were purchased in pharmaceutical or cosmetic grade, as applicable.
The color-imparting agents were generally purchased from Jarocol.
The tablet ingredients (including color-imparting agents) were mixed together.
Before mixing, one of the tablet ingredients was optionally ground with a cutting mill (Fritsch Pulverisette 19, with a 250 micron insert sieve) under operating conditions, to obtain a similar size distribution for all the ingredients of compressed. In a representative procedure, for a 400 gram block, the ingredients were ground for about 2 hours at a power of 2,000 W, although longer times can be used for ingredients made of hard bulk material and / or having large initial size. they were inevitably ground for up to 4 hours.
The obtained particles were then optionally sieved by means of release techniques with meshes having apertures of 212 μm, 150 μm and 45 μm (Retsch AS 200 vibrating sieve shaker) to obtain predominantly particles having a size ranging from 45 μm to 150 μm .
The tablet ingredients, whether or not ground and / or sieved, were then transferred to an oven set at 50 ° C to homogeneously dry the particles. After 24 hours, desired amounts of the dry particles of the various tablet ingredients were thoroughly mixed for at least 20 minutes using a motorized V-shaped mixer (model GHJ-10V, Jiangyin Longchang Machinery Manufacture Co.).
The pulverized mixture obtained was then compressed into a tablet, using either a manual or an automatic tableting machine.
In the manual tableting setup, 1.5 kg of the mixture was fed into an AISI 316 stainless steel cylinder having a diameter of about 25 mm. The corresponding piston was placed on the pulverized mixture, which was then compressed with a manual hydraulic press (Mazzola, W20) applying a pressure of 25 N on the resulting tablet, which had an average thickness of about 3 mm.
A 10 station rotary tablet press machine (TPC-10-B, Dynamic Exim Corp.) was used for the automated process, with modified ball configuration tooling having a diameter of 4.5mm or 5.0mm. (iHolland). The modified ball punches were adjusted to allow the production of tablets having a maximum thickness similar to the tablet diameter, hence for the preparation of approximately spherical tablets having a diameter of 4.5mm or 5.0mm.
The average weight of a 5.0 mm spheroid tablet commonly ranged from about 70 mg to about 90 mg, depending on the formulation used.
The applied compression was generally between 5 kN and 7.5 kN for a single point punch, generally resulting in a hardness of 3.0 kgf to 5.0 kgf (as further detailed in Example 3 below). in the present document).
Tablet formulations:
Using the methods described above, several tablets were prepared. Tables 1A to 1C below present the composition of the tablet with the percentage by weight of each component of the total weight of an uncoated tablet. Table 1A presents control tablet compositions devoid of color-imparting agents, which are also referred to herein as placebo tablets; Table 1B presents basic shade tablet compositions comprising (color-imparting agents that are prepared at both about 4.5 and 5.0 mm diameter). And Table 1C presents rapid disintegration media tablet compositions comprising oxidizing agents (see tablets # 201-204), thickening agents (see tablets # 205-208) and alkaline agents (see tablets # 209). ).
The various grades of Avicel® (FMC Corporation) and Comprecel correspond to various types of microcrystalline cellulose; the GalenlG ™ (Palatinit) and Isomalt ™ grades correspond to various isomalt preparations; LH-21 and LH-22 (Shin Etsu) are types of low substituted hydroxypropyl cellulose (HPC); Ludiflash® (BASF) and Parteck® M and ODT grades are mannitol-based, while Parteck® SI grades (Merck) are sorbitol-based and PEO N-IO (DOW) is a polyethylene oxide. Ludiflash® comprises in addition to mannitol, PVA, PVP and polyvidone. SuperTab® IlSD is a dry atomized form of lactose and all of the previously mentioned ingredients of Avicel® or SuperTab® serve alone or in combination as global excipients (e.g., binder, filler), although some of them may
ES 2 823 977 T3 can also be considered as auxiliary disintegrants (eg, LH-21, LH-22, SuperTab® IlSD). AC-Di-sol® SD711 is a type of croscarmellose sodium, Polyplasdone® (ISP) grades correspond to various types of cross-linked polyvinylpyrrolidone and Primojel® comprises sodium starch glycolate. The last group of ingredients serves as a disintegrant envelope. A third series of ingredients serve as additives such as antioxidants (ascorbic acid) and lubricants / release agents / slip agents (magnesium stearate, Alubra ™, comprising sodium stearyl fumarate and Parteck® LUB CST, LUB MST and LUB STA 50 from Merck, which respectively comprise calcium stearate, magnesium stearate and stearic acid).
Formulations made without lubricants were manually compressed. Such formulations were adapted to automatic tableting by adding a lubricant (eg, 1% Mg stearate or any other appropriate amount of appropriate ingredient) and decreasing the overall amount of excipient by the same amount.
Some basic tone tablets were prepared in two versions, one comprising only dye precursors and couplers and another comprising the same precursors and couplers in the same amount together with direct dyes, in which case the overall excipient amount was decreased accordingly. . The version with the direct dyes is presented in Table 1B, the version without the direct dye is denoted by the same number of tablets followed by an apostrophe (for example, tablet 103 corresponds to the red tone comprising 0.08% red HC No. 10 and 11, while tablet No. 103 'corresponds to a red shade that lacks such direct dyes and comprises 60.5% Avicel® PH-102).
Table 1A
<td>Tablet # Ingredient</td><td> 1</td><td> 2</td><td> 3</td><td> 4</td><td> 5</td><td> 6</td><td> 7</td><td> 8</td>
<td>Avicel® CE-15</td><td> 99,50</td><td> 99,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® HFE-102</td><td> -</td><td> -</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® PH-101</td><td> -</td><td> -</td><td> -</td><td> 99,00</td><td> 99,00</td><td> 64,50</td><td> 64,50</td><td> 64,50</td>
<td>SuperTab® 11SD</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 33,00</td><td> 33,00</td><td> 33,00</td>
<td>AC-Di-Sol® SD711</td><td> 0,50</td><td> -</td><td> 0,50</td><td> -</td><td> -</td><td> 2,00</td><td> 2,00</td><td> 2,00</td>
<td>Polyplasdone® INF-10</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Polyplasdone® XL</td><td> -</td><td> 1,00</td><td> -</td><td> 1,00</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Polyplasdone® XL-10</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> -</td><td> -</td><td> -</td>
<td>Parteck® LUB CST</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,50</td><td> -</td><td> -</td>
<td>Parteck® LUB MST</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,50</td><td> -</td>
<td>Parteck® LUB STA 50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,50</td>
<td>Tablet # Ingredient</td><td> 9</td><td> 10</td><td> 11</td><td> 12</td><td> 13</td><td> 14</td><td> 15</td><td> 16</td>
<td>Avicel® PH-101</td><td> 65,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® PH-102</td><td> -</td><td> 70,00</td><td> 70,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® PH-102 SCG</td><td> -</td><td> -</td><td> -</td><td> 99,50</td><td> 99,00</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® PH-105</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 99,00</td><td> 99,00</td><td> 99,00</td>
<td>SuperTab® 11SD</td><td> 33,00</td><td> 27,00</td><td> 22,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>AC-Di-Sol® SD711</td><td> 2,00</td><td> 2,00</td><td> 2,00</td><td> 0,50</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Polyplasdone® INF-10</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> -</td><td> -</td>
<td>Polyplasdone® XL</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> -</td><td> 1,00</td><td> -</td>
<td>Polyplasdone® XL-10</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td>
<td>Ascorbic acid</td><td> -</td><td> -</td><td> 5,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Magnesium stearate</td><td> -</td><td> 1,00</td><td> 1,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
ES 2 823 977 T3
<td>Tablet # Ingredient</td><td> 17</td><td> 18</td><td> 19</td><td> 20</td><td> 21</td><td> 22</td><td> 23</td><td> 24</td>
<td>Avicel® PH-105</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® PH-200</td><td> -</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Avicel® PH-301</td><td> -</td><td> -</td><td> 99,50</td><td> 99,00</td><td> 99,00</td><td> 97,50</td><td> -</td><td> -</td>
<td>Avicel® PH-302</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 99,50</td><td> 99,00</td>
<td>AC-Di-Sol® SD711</td><td> 0,50</td><td> 0,50</td><td> 0,50</td><td> -</td><td> -</td><td> 0,50</td><td> 0,50</td><td> -</td>
<td>Polyplasdone® XL</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> -</td><td> -</td><td> -</td><td> 1,00</td>
<td>Polyplasdone® XL-10</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> 2,00</td><td> -</td><td> -</td>
<td>Tablet # Ingredient</td><td> 25</td><td> 26</td><td> 27</td><td> 28</td><td> 29</td><td> 30</td><td> 31</td><td> 32</td>
<td>Avicel® PH-302</td><td> 99,00</td><td> 97,00</td><td> 97,50</td><td> 65,00</td><td> 70,00</td><td> -</td><td> -</td><td> -</td>
<td>Comprecel M101</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 97,00</td><td> 99,50</td><td> -</td>
<td>Comprecel M102</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 97,00</td>
<td>GalenIQ ™ 721</td><td> -</td><td> -</td><td> -</td><td> 34,50</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>SuperTab® 11SD</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 27,00</td><td> -</td><td> -</td><td> -</td>
<td>AC-Di-sol® SD711</td><td> -</td><td> -</td><td> 0,50</td><td> 0,50</td><td> 2,00</td><td> -</td><td> 0,50</td><td> -</td>
<td>Polyplasdone® XL</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 3,00</td><td> -</td><td> 3,00</td>
<td>Polyplasdone® XL-10</td><td> 1,00</td><td> 3,00</td><td> 2,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Magnesium stearate</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> -</td><td> -</td><td> -</td>
<td>Tablet # Ingredient</td><td> 33</td><td> 34</td><td> 35</td><td> 36</td><td> 37</td><td> 38</td><td> 39</td><td> 40</td>
<td>Comprecel M102</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>GalenlQ ™ 720</td><td> -</td><td> 97,00</td><td> 99,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>GalenlQ ™ 721</td><td> -</td><td> -</td><td> -</td><td> 97,00</td><td> 99,00</td><td> -</td><td> -</td><td> -</td>
<td>GalenlQ ™ 800</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 97,00</td><td> 99,00</td><td> -</td>
<td>GalenlQ ™ 810</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 97,00</td>
<td>AC-Di-sol® SD711</td><td> 0,50</td><td> -</td><td> 1,00</td><td> -</td><td> 1,00</td><td> -</td><td> 1,00</td><td> -</td>
<td>Polyplasdone® INF-10</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Polyplasdone® XL</td><td> -</td><td> 3,00</td><td> -</td><td> 3,00</td><td> -</td><td> 3,00</td><td> -</td><td> 3,00</td>
Table 1A (continued)
<td>Tablet # Ingredient</td><td> 41</td><td> 42</td><td> 43</td><td> 44</td><td> 45</td><td> 46</td><td> 47</td><td> 48</td>
<td>GalenlQ ™ 810</td><td> 99,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>GalenlQ ™ 960</td><td> -</td><td> 97,00</td><td> 99,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Isomalt ™ GS</td><td> -</td><td> -</td><td> -</td><td> 75,40</td><td> 43,40</td><td> -</td><td> -</td><td> -</td>
<td>LH-21 (HPC)</td><td> -</td><td> -</td><td> -</td><td> 9,60</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>LH-22 (HPC)</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 48,00</td><td> -</td><td> -</td><td> -</td>
ES 2 823 977 T3
<td>Ludiflash®</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 100,0</td><td> -</td><td> -</td>
<td>Parteck® Delta M</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 99,50</td><td> -</td>
<td>Parteck® M 100</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 99,50</td>
<td>PEO N-10</td><td> -</td><td> -</td><td> -</td><td> 15,00</td><td> 8,60</td><td> -</td><td> -</td><td> -</td>
<td>AC-Di-sol® SD711</td><td> 1,00</td><td> -</td><td> 1,00</td><td> -</td><td> -</td><td> -</td><td> 0,50</td><td> 0,50</td>
<td>Polyplasdone® XL</td><td> -</td><td> 3,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Tablet # Ingredient</td><td> 49</td><td> 50</td><td> 51</td><td> 52</td><td> 53</td><td> 54</td><td> 55</td><td> 56</td>
<td>Avicel® PH-102</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 69,60</td><td> 70,40</td>
<td>Parteck® M 200</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Parteck® ODT</td><td> -</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Parteck® Sl 200</td><td> -</td><td> -</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Parteck® Sl 400</td><td> -</td><td> -</td><td> -</td><td> 99,50</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Parteck® Sl 450</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 99,50</td><td> -</td><td> -</td><td> -</td>
<td>SuperTab® 11SD</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 97,00</td><td> 26,40</td><td> 26,60</td>
<td>AC-Di-SOl® SD711</td><td> 0,50</td><td> 0,50</td><td> 0,50</td><td> 0,50</td><td> 0,50</td><td> 2,00</td><td> -</td><td> 2,00</td>
<td>Primojel®</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 3,00</td><td> -</td>
<td>Alubra<sup>TM</sup> PG-100</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td>
<td>Magnesium stearate</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,00</td><td> 1,00</td><td> -</td>
Table 1B
<td>Tablet # Ingredient</td><td> 101</td><td> 102</td><td> 103</td><td> 104</td><td> 105</td><td> 106</td><td> 107</td><td> 108</td><td> 109</td>
<td>Tone</td><td>rose</td><td>Orange</td><td>Red</td><td>OR ω or Q</td><td>purple</td><td>Blue</td><td>Ash</td><td>natural</td><td>Green</td>
<td>Avicel® PH-102</td><td> 67,71</td><td> 63,32</td><td> 60,43</td><td> 67,50</td><td> 58,87</td><td> 63,01</td><td> 68,93</td><td> -</td><td> 60,70</td>
<td>Avicel® PH-200</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 58,74</td><td> -</td>
<td>SuperTab® 11SD</td><td> 25,63</td><td> 23,96</td><td> 22,90</td><td> 25,54</td><td> 22,33</td><td> 23,85</td><td> 26,09</td><td> 22,23</td><td> 23,17</td>
<td>AC-Di-sol® SD711</td><td> 2,00</td><td> 2,00</td><td> 3,00</td><td> 2,00</td><td> 3,00</td><td> 2,00</td><td> 2,00</td><td> 2,00</td><td> 2,00</td>
<td>Magnesium stearate</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td>
<td>Ascorbic acid</td><td> 1,00</td><td> 1,00</td><td> 3,00</td><td> 1,00</td><td> 3,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td>
<td>p-aminophenol</td><td> 1,17</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>4-amino-m-cresol</td><td> -</td><td> 0,30</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>1-Hydroxyethyl-4,5-diamino pyrazole sulfate</td><td> -</td><td> -</td><td> 6,30</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>N, n-bis (2-hydroxy-ethyl) -p-phenylene-diamine sulfate</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 8,30</td><td> 4,96</td><td> -</td><td> -</td><td> -</td>
<td>Toluene-2,5-diamine sulfate</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,50</td><td> 10,13</td><td> 3,80</td>
<td>4-amino-2-hydroxytoluene</td><td> 1,50</td><td> 0,30</td><td> 3,30</td><td> -</td><td> 3,50</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>2,4-diamino-phenoxy-ethanol diHCI</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 4,04</td><td> 0,40</td><td> -</td><td> -</td>
<td>m-aminophenol</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,47</td><td> -</td>
<td>Resorcinol</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 4,43</td><td> -</td>
<td>Hydroxyethyl-3,4-methylene dioxyaniline HCl</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,10</td><td> -</td><td> 3,80</td>
<td>2-amino-6-chloro-4-nitrophenyl l</td><td> -</td><td> 8,14</td><td> -</td><td> 3,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
ES 2 823 977 T3
<td>HC Red # 10 & 11</td><td> -</td><td> -</td><td> 0,08</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>HC Blue # 15</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,16</td><td> -</td><td> -</td><td> 0,03</td>
<td>HC Yellow # 13</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 4,00</td>
<td>2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,50</td>
Table 1C
<td>Tablet # Ingredient</td><td> 201</td><td> 202</td><td> 203</td><td> 204</td><td> 205</td><td> 206</td><td> 207</td><td> 208</td><td> 209</td>
<td>Urea Hydrogen Peroxide</td><td> 35,00</td><td> 97,00</td><td> 50,00</td><td> 50,00</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Carbopol® Ultrez 20</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 10,00</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Stabileze® QM</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 6,00</td><td> 7,00</td><td> 12,00</td><td> -</td>
<td>(NH4) 2CO3</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 30,00</td>
<td>Avicel® ΡΗ 102</td><td> -</td><td> -</td><td> 47,00</td><td> 34,10</td><td> 53,60</td><td> 65,30</td><td> 63,10</td><td> 59,50</td><td> 48,60</td>
<td>SuperTab® 11SD</td><td> 62,00</td><td> -</td><td> -</td><td> 12,90</td><td> 20,30</td><td> 24,70</td><td> 23,90</td><td> 22,50</td><td> 18,40</td>
<td>AC-Di-sol® SD711</td><td> 2,00</td><td> 2,00</td><td> 2,00</td><td> 2,00</td><td> 2,00</td><td> 3,00</td><td> -</td><td> -</td><td> 2,00</td>
<td>Polyplasdone® XL</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 5,00</td><td> 5,00</td><td> -</td>
<td>Ascorbic acid</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 7,00</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Sodium bicarbonate</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 6,10</td><td> -</td><td> -</td><td> -</td><td> -</td>
<td>Magnesium stearate</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td><td> 1,00</td>
Tables 1D and 1E present exemplary improved formulations prepared in order to allow accurate coloring and analysis with an algorithm system as described herein, by containing a color-imparting agent.
The ratio of the oxidation dye precursor to the coupler was finely adjusted (being less than 1) in order to avoid the possible formation of harmful compounds.
Table 1D
<td>Tablet # Ingredient</td><td> 1</td><td> 2</td><td> 3</td><td> 4</td><td> 5</td><td> 6</td><td> 7</td><td> 8</td><td> 9</td>
<td>Tone</td><td>natural</td><td>Golden</td><td>Orange</td><td>Red</td><td>purple</td><td>Ash</td><td>rose</td><td>Green</td><td>Blue</td>
<td>Avicel® PH-200</td><td> 58,9 %</td><td> 68,5 %</td><td> 60,5 %</td><td> 60,4 %</td><td> 57,8 %</td><td> 68,8 %</td><td> 69,1 %</td><td> 61,2 %</td><td> 61,3 %</td>
<td>SuperTab® 11SD</td><td> 22,2 %</td><td> 25,9 %</td><td> 22,9 %</td><td> 22,9 %</td><td> 22 %</td><td> 26,2 %</td><td> 26,2 %</td><td> 23,1 %</td><td> 23,2 %</td>
<td>AC-Di-sol® SD711</td><td> 2 %</td><td> 2 %</td><td> 2 %</td><td> 3 %</td><td> 3 %</td><td> 2 %</td><td> 2 %</td><td> 2 %</td><td> 2 %</td>
<td>Magnesium stearate</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 3 %</td><td> 3 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td>
<td>Ascorbic acid</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td>
<td>Toluene-2,5-diamine sulfate</td><td> 9,93 %</td><td></td><td></td><td></td><td></td><td> 0,24 %</td><td></td><td> 3,8 %</td><td></td>
ES 2 823 977 T3
<td>1-Hydroxyethyl-4,5-diamino-pyrazole sulfate</td><td></td><td></td><td></td><td> 6,3 %</td><td></td><td></td><td></td><td></td><td></td>
<td>N, N-bis (2-hydroxyethyl) -p-phenylenediamine sulfate</td><td></td><td></td><td></td><td></td><td> 9,25 %</td><td></td><td></td><td></td><td> 6,2 %</td>
<td>4-amine-m-cresol</td><td></td><td></td><td> 0,43 %</td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>p-aminophenol</td><td></td><td></td><td></td><td></td><td></td><td></td><td> 0,35 %</td><td></td><td></td>
<td>4-amino-2-hydroxytoluene</td><td></td><td></td><td> 0,43 %</td><td> 3,3 %</td><td> 3,9 %</td><td></td><td> 0,45 %</td><td></td><td></td>
<td>2,4-diamino-phenoxy-ethanol 2HCl</td><td></td><td></td><td></td><td></td><td></td><td> 0,22 %</td><td></td><td></td><td> 5,05 %</td>
<td>m-aminophenol</td><td> 0,91 %</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>Resorcinol</td><td> 4,05 %</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>Hydroxyethyl-3,4-methylene-dioxyaniline HCl</td><td></td><td></td><td></td><td></td><td></td><td> 0,46 %</td><td></td><td> 3,8 %</td><td></td>
<td>2-amino-6-chloro-4-nitrophenol</td><td></td><td> 1,55 %</td><td> 11,7 %</td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>HC Red # 10 & 11</td><td></td><td></td><td></td><td> 0,075 %</td><td></td><td></td><td></td><td></td><td></td>
<td>HC Yellow # 13</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td> 4 %</td><td></td>
<td>2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>HC Blue # 15</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td> 0,03 %</td><td> 0,2 %</td>
Table 1E
<td>Tablet # Ingredient</td><td> 10</td><td> 11</td><td> 12</td><td> 13</td><td> 14</td><td> 15</td><td> 16</td><td> 17</td><td> 18</td>
<td>Tone</td><td>natural</td><td>Golden</td><td>Orange</td><td>Red</td><td>purple</td><td>Ash</td><td>rose</td><td>Green</td><td>Blue</td>
<td>Avicel® PH-102</td><td> 58,9 %</td><td> 68,5 %</td><td> 60,5 %</td><td> 60,4 %</td><td> 57,8 %</td><td> 69,3 %</td><td> 69,1 %</td><td> 63,9 %</td><td> 61,3 %</td>
<td>SuperTab® 11SD</td><td> 22,2 %</td><td> 25,9 %</td><td> 22,9 %</td><td> 22,9 %</td><td> 22 %</td><td> 26,2 %</td><td> 26,2 %</td><td> 23,1 %</td><td> 23,2 %</td>
<td>AC-Di-sol® SD711</td><td> 2 %</td><td> 2 %</td><td> 2 %</td><td> 3 %</td><td> 3 %</td><td> 2 %</td><td> 2 %</td><td> 2 %</td><td> 2 %</td>
<td>Magnesium stearate</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 3 %</td><td> 3 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td>
<td>Ascorbic acid</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td><td> 1 %</td>
<td>Toluene-2,5-diamine sulfate</td><td> 9,93 %</td><td></td><td></td><td></td><td></td><td> 0,24 %</td><td></td><td> 3,46 %</td><td></td>
<td>1-Hydroxyethyl-4,5-diamino-pyrazole sulfate</td><td></td><td></td><td></td><td> 6,3 %</td><td></td><td></td><td></td><td></td><td></td>
<td>N, N-bis (2-hydroxyethyl-pphenylenediamine) sulfate</td><td></td><td></td><td></td><td></td><td> 9,25 %</td><td></td><td></td><td></td><td> 6,2 %</td>
<td>4-amine-m-cresol</td><td></td><td></td><td> 0,43 %</td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>p-aminophenol</td><td></td><td></td><td></td><td></td><td></td><td></td><td> 0,35 %</td><td></td><td></td>
<td>• 4-amino-2-hydroxytoluene</td><td></td><td></td><td> 0,43 %</td><td> 3,3 %</td><td> 3,9 %</td><td></td><td> 0,45 %</td><td></td><td></td>
ES 2 823 977 T3
<td>2,4-diamino-phenoxy-ethanol 2HCl</td><td></td><td></td><td></td><td></td><td></td><td> 0,22 %</td><td></td><td></td><td> 5,05 %</td>
<td>m-aminophenol</td><td> 0,91 %</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>Resorcinol</td><td> 4,05 %</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>Hydroxyethyl-3,4-methylene-dioxyaniline HCl</td><td></td><td></td><td></td><td></td><td></td><td> 0,46 %</td><td></td><td> 3,43 %</td><td></td>
<td>2-amino-6-chloro-4-nitrophenol</td><td></td><td> 1,55 %</td><td> 11,7 %</td><td></td><td></td><td></td><td></td><td></td><td></td>
<td>HC Red # 10 & 11</td><td></td><td></td><td></td><td> 0,075 %</td><td></td><td></td><td></td><td></td><td></td>
<td>HC Yellow # 13</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td> 2 %</td><td></td>
<td>2,6-diamino-3 - ((pyridin-3-yl) azo) pyridine</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td> 0,025 %</td><td></td>
<td>HC Blue # 15</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td> 0,025 %</td><td> 0,2 %</td>
<td>Base / ratio coupled</td><td> 0,99</td><td> -</td><td> 0,99</td><td> 0,98</td><td> 0,93</td><td> 0,99</td><td> 0,87</td><td> 0,99</td><td> 0,95</td>
Tables 1D and 1E each present a combination of exemplary formulations for a variety of basic shades, which can be combined to form a wide variety of shades. Exemplary formulations comprise, as color-imparting agents, a combination of one or more dye precursors with one or more dye couplers and / or one or more direct dyes. The dye precursors used include toluene-2,5-diamine, 1-hydroxyethyl-4,5-diamino-pyrazole, N, N-bis (2-hydroxyethyl) -p-phenylene-diamine, 4-amino-m-cresol and p -aminophenol. The dye couplers used include 4-amino-2-hydroxytoluene, 2,4-diamino-phenoxy-ethanol, m-aminophenol, resorcinol, and hydroxyethyl-3,4-methylene-dioxyaniline. Direct dyes used include 2-amino-6-chloro-4-nitrophenol, HC red # 10 and 11, HC yellow # 13, 2,6-diamino-3 ((pyridin-3-yl) azo) pyridine and HC blue # 15).
In the formulation presented in Table 1E, the molar ratio between the basic dye (dye precursor) and the dye coupler was finely controlled not to exceed 1.0.
EXAMPLE 2
Tablet coatings
Tablets prepared as described in Example 1 were, where desired, further coated, for example, to improve the hardness of the tablets, reduce the penetration of undesirable oxygen and / or moisture, and extend the shelf life of the tablets.
The tablets were spray coated using a perforated tray coater (Freund Vecor, Laboratory LDCS-Hi Costers®) with a 2.5 I electro polished fully perforated tray. Coating solutions were generally sprayed using the Shlick ABC spray gun at an average inlet temperature of 74-77 ° C and an average exhaust temperature of 45-50 ° C for up to 105 minutes, depending on the concentration of the coating. coating solution, atomization rate and desired thickness. The thickness of the resulting coatings was finished by cutting the tablet and measuring the coating thickness in the resulting cross section under an optical microscope (Olympus BX51). The average thickness reported is the average of four measurements made on two tablets from the same batch. Alternatively, the coating thickness could be estimated according to the weight gained by the tablet following the coating, by approximating the shape of the tablet to a sphere. Assuming that the coating and the tablet have the same density, the weight increase percent of the AW tablet, given by equation 1, allows the estimation of the thickness r2-ri, where n is the initial radius of the uncoated tablet and r2 is the final radius of the coated tablet:
lOOM — P [<sub>Ec</sub> η
X <sup>r</sup>l /
The percent weight gain presented in Table 2A is calculated by equating the weight gain of the tablets to the weight of the applied coating. In Table 2B it is calculated by measuring the weight of 100 tablets before and after coating using an analytical weight (ML204 / 01, Mettler Toledo).
Coating solutions were prepared by dissolving the coating agent of interest in deionized water,
ES 2 823 977 T3 commonly by stably adding the powder to a vortex formed by a propellant stirrer (Ultra-Turrax® T50 Basic with accessories from R 1402 Dissolver, Ika Werke). Once all the powder was added, the propellant speed was reduced from 2,000 RPM to 500 RPM, which nearly eliminated the vortex and the solution was further mixed for 30 minutes. Coating agents, when applicable with color identifiers, were purchased pharmaceutical or edible grade. Opadry® coatings were obtained from Colorcon and Kollicoat® coatings were obtained from BASF. These coatings were generally based on hydroxy propyl methyl cellulose (HPMC), polyethylene glycol (PEG), polyvinyl alcohol (PVA), polyvinyl alcohol polyethylene glycol graft copolymer (PVA-PEG), or mixtures thereof. Rapid Subcoat sD-9600, based on sucrose, pEg and xanthan gum was purchased from Colorcon and used at a concentration of 5%. Inlet temperatures of around 74 ° C were commonly used for coatings based on sucrose, HPMC and PVA-PEG copolymers and inlet temperatures of around 77 ° C were used for coatings based on pVa.
1.2-1.6 kg batches of desired tablets were fed into the 2.5 liter perforated tray which was rotated at 18 RPM. The contents of the tray were heated by the incoming hot air and the temperature of the exhaust air was monitored as an indicator of the temperature of the tablets. Once the tablets were preheated to around 45-50 ° C, coating solutions were peristaltically pumped into the system at the desired speed and generally atomized at an air flow rate of 90-100 m.<sup>3</sup>/ hour with a spray gun atomization pressure of 70 to 90 kPa (700 to 900 mbar) and an air pattern of 100 to 160 kPa (1,000 to 1,600 mbar). Several coated tablets were prepared by this method, including control tablets devoid of color-imparting agents. The compositions of the coating solutions (in percent by weight of the total weight of the coating solution), the atomization rate of the coating solution (in grams / minute), the duration of the coating (in minutes), the contribution final coating solids (as weight percent uncoated tablet) and the measured or calculated thickness of the resulting coatings (in microns) are presented in Tables 2A and 2B.
The coating experiments reported in Table 2A were performed at a coating rate of about 7 grams / minute, except for coatings # 4.8 and 12 which were prepared at a rate of about 4 grams / minute. In additional experiments reported in Table 2B, the coating solutions were sprayed for about 45 minutes at a rate of 9-10 g / min. The coating thicknesses reported in table 2A were measured using optical microscopy and in table 2B they were both measured and calculated according to equation 1.
Table 2A
<td>Coating No.</td><td> 1</td><td> 2</td><td> 3</td><td> 4</td><td> 5</td><td> 6</td><td> 7</td><td> 8</td><td> 9</td><td> 10</td><td> 11</td><td> 12</td>
<td>HPMC Blue Opadry® Il</td><td> 5 %</td><td> -</td><td> -</td><td> -</td><td> 5 %</td><td> -</td><td> -</td><td> -</td><td> 5 %</td><td> -</td><td> -</td><td> -</td>
<td>Yellow PVA Opadry® Il</td><td> -</td><td> 5 %</td><td> -</td><td> -</td><td> -</td><td> 5 %</td><td> -</td><td> -</td><td> -</td><td> 5 %</td><td> -</td><td> -</td>
<td>Brilliant blue IR Kollicoat®</td><td> -</td><td> -</td><td> 5 %</td><td> 1 %</td><td> -</td><td> -</td><td> 5 %</td><td> 1 %</td><td> -</td><td> -</td><td> 5 %</td><td> 1 %</td>
<td>Protect Kollicoat®</td><td> -</td><td> -</td><td> -</td><td> 4 %</td><td> -</td><td> -</td><td> -</td><td> 4 %</td><td> -</td><td> -</td><td> -</td><td> 4 %</td>
<td>Coating duration (min)</td><td colspan="4"> 75</td><td colspan="4"> 90</td><td colspan="4"> 105</td>
<td>Coating amount (% by weight)</td><td> 2,1</td><td> 2,1</td><td> 2,1</td><td> 1,3</td><td> 2,6</td><td> 2,6</td><td> 2,6</td><td> 1,5</td><td> 3,0</td><td> 3,0</td><td> 3,0</td><td> 1,8</td>
<td>Coating thickness (μm)</td><td> 15</td><td> 13</td><td> 17</td><td> 10</td><td> 20</td><td> 19</td><td> 23</td><td> 12</td><td> 25</td><td> 24</td><td> 25</td><td> 15</td>
ES 2 823 977 T3
Table 2B
<td>Coating No.</td><td> 13</td><td> 14</td><td> 15</td><td> 16</td><td> 17</td><td> 18</td><td> 19</td><td> 20</td><td> 21</td>
<td>Black IR Kollicoat®</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 0,1 %</td><td> -</td><td> -</td>
<td>Carmine IR Kollicoat®</td><td> 0,4 %</td><td> 0,3 %</td><td> -</td><td> -</td><td> -</td><td> 0,15 %</td><td> -</td><td> -</td><td> -</td>
<td>IR white Kollicoat®</td><td> 0,6 %</td><td> 0,4 %</td><td> -</td><td> 0,7 %</td><td> -</td><td> -</td><td> 0,7 %</td><td> -</td><td> 0,6 %</td>
<td>Sunset Yellow IR Kollicoat®</td><td> -</td><td> 0,3 %</td><td> 1 %</td><td> 0,3 %</td><td> -</td><td> -</td><td> -</td><td> 0,75 %</td><td> 0,2 %</td>
<td>Brilliant blue IR Kollicoat®</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1 %</td><td> 0,85 %</td><td> 0,2 %</td><td> 0,25 %</td><td> 0,2 %</td>
<td>Protect Kollicoat®</td><td> 4 %</td><td> 4 %</td><td> 4 %</td><td> 4 %</td><td> 4 %</td><td> 4 %</td><td> 4 %</td><td> 4 %</td><td> 4 %</td>
<td>Coating amount (% by weight)</td><td> 1,60</td><td> 1,70</td><td> 1,62</td><td> 1,79</td><td> 1,95</td><td> 1,64</td><td> 1,74</td><td> 1,56</td><td> 1,78</td>
<td>Average coating thickness (μm)</td><td> 17</td><td> 16</td><td> 18</td><td> 18</td><td> 21</td><td> 16</td><td> 13</td><td> 15</td><td> 17</td>
<td>Calculated coating thickness (μm)</td><td> 13</td><td> 14</td><td> 13</td><td> 15</td><td> 16</td><td> 14</td><td> 14</td><td> 13</td><td> 15</td>
The variation in the average weight of the coated tablets was at most 10% for tablets of a given batch formulation. This variability, however, which results from the coating process, does not affect the accuracy of the doses, since the core tablets that provide the desired color-imparting agents or other active ingredients (e.g. alkaline agents, oxidizers, bleaches , thickeners) have a very low deviation from the average weight of each fast-disintegrating tablet or tone (ie less than 2%).
In order to improve the number of appropriate coating colors and in order to obtain this stability of a coating towards UV light, alternative coating procedures were developed.
The coating used the following aqueous coating formulation: 4% (w / w) polyvinyl alcohol (IR Kollicoat coating polymer, BASF); synthetic pigment 1% (w / w) and 95% water. The polyvinyl alcohol and pigments were mixed together in powder form and then added to stirred water by an IKAT-50 homogenizer equipped with a 1402 dissolving tool to obtain an aqueous coating solution.
The tablets were coated by spraying the aqueous solution onto uncoated (core) tablets. Representative examples of tablets coated by these procedures are shown in Figures 10A and 10B.
The thickness of the tablet coating was determined using a light microscope and camera programming element analysis, as described in Example 2. A representative image of a coated tablet is shown in Figure 11. Five tablets of formulation n. 14 (see Table 1E) were sampled and the thickness was determined at 10 sites for each tablet.
As shown in Figure 12, the experiment exhibited an average thickness of 13.12 microns, the average thickness of each of the 10 tablets tested is in a range of about 11-17 microns.
These results indicate that the coating procedure provides a reasonably uniform tablet coating.
EXAMPLE 3
Tablet properties
ES 2 823 977 T3
Coated and uncoated tablets prepared as described in Examples 1 and 2 were subjected to numerous tests to determine certain properties.
Mechanical properties were measured using a tablet hardness tester (HT-50P), a friable tester (FTA-20), and a disintegration tester (TD-20S) all from Thermonik Campbell Electronics. These properties were determined at various points in time following tabletting.
The stability of the tablets was determined under normal and accelerated conditions. Accelerated conditions were produced by incubating the tested tablets in an environmental chamber (KBF115, Binder). The tablets were removed from the environmental chamber after different durations and their performance over time was compared to established reference values following closely tabletting and / or coating (time point 0). Unless stated otherwise, the environmental chamber maintained a stable temperature of 25 ° C and relative humidity of 65% (RH).
The chemical stability of the color-imparting agents was determined by scanning spectrometry (UV-Visible Cary 300 Agilent Technologies spectrophotometer).
As a rule, at least three tablets were used for each test and / or the test was repeated. To determine the hardness, a tablet was placed in the tester until the tablet breaks. The reported value indicates the force required to break the tablet. To determine the friable, 10 tablets were inserted into the chamber of the tester, which was then rotated 25 times at a speed of 25 rpm. The tablet weights before and after the test were analytically measured and compared, the friable value is the percent weight loss.
To determine disintegration, the tablets were placed in a perforated basket which was moved up and down at constant speed in a beaker containing 500 ml of test medium at room temperature of about 25 ° C. The time to total disintegration was measured. When disintegration was tested in a non-viscous medium, total disintegration was adjusted to occur when no visible fragment of the tablet remains in the basket. When tested in a viscous medium, the swollen tablets may not spontaneously pass through the mesh of the basket and total disintegration was adjusted to occur when no fragment of the tablets remains in the basket. When tested in a viscous medium, the swollen tablets may not spontaneously pass through the mesh of the basket and total disintegration was adjusted to occur when no fragment of the tablets remains in the basket after an operator gently squeezed the swollen tablet. through the mesh (that is, no core remaining).
The medium used to test the disintegration rate was either deionized water (pH 7.0, 1 cP viscosity) or a commercially available hydrogen peroxide emulsion (6% H2O2, pH 3.0, viscosity less than 0.5 poise) or an emulsion of hydrogen peroxide (Welloxon 9% H2O2) diluted at a ratio of 30:70 wt with deionized water (final viscosity 0.5 poise, pH 4.0). It should be noted that the disintegration time was determined without manual mixing. Therefore, the durations reported below represent upper limits that are expected to be reduced by further mixing. To determine the chemical stability of the dyes, a tablet was dissolved in 250 ml of deionized water and a 2 ml sample was transferred in a quartz cuvette to the spectrophotometer. The volume of solution was selected to obtain an optical density of at most about 1.
A first set of experiments, control tablets containing 70% microcrystalline cellulose pH 102 from Avicel®, 27% spray dried lactose SuperTab® 11SD, 2% croscarmellose sodium Ac-Di-Sol® SD711 and 1% stearate magnesium were tested before and after coating. Coating solutions were prepared at a concentration of 5% in deionized water and sprayed at a similar rate of 6.8 grams / minute, with the exception of Coating B which was sprayed at about 4.1 grams / minute. The coating agents tested were Brilliant Blue Kollicoat®, Brilliant Blue IR Kollicoat® + Protector Kollicoat® (1% + 4%) and Opadry® II coatings based on either HPMC or PVA, respectively A, B, C and D in Table 3A. Tablets were sampled every 15 minutes up to 105 minutes of coating.
Additional experiments are reported in Table 3B, the number of tablets refers to the information provided in Table 1B in Example 1 and the coating number refers to the information provided in Example 2. For reference, the disintegration time for the uncoated versions of these tablets in water it was less than 30 seconds for all basic shade tablets. The friability of the coated basic shades was established at the zero time point and the chemical stability was monitored for the duration of the preliminary environmental chamber test. All shades were tested for at least 5 days.
Tables 3A and 3B report the properties of tablets measured by these methods. Points in time are given in days, weeks, or months, as the case may be. The hardness is given in kgf, the friability is
ES 2 823 977 T3 given in percent weight loss, the friable time is given in seconds (table 3A) or minutes: seconds (table 3B). For reference, all uncoated versions of the reported tablets had reference hardness between 2.0 and 4.5 kgf. When applicable, the chemical stability is given as 0 or 1, where 1 means a spectrum identical or almost identical to the reference spectrum and 0 means the spectrum where the maximum 5 of the dyes have reduced area and / or have disappeared and / or it has moved out of position and / or new highs have appeared. Stability graduated as 0 and both the optical spectrum are concerned and may not necessarily mean that residual dyes cannot obtain hair coloring to some extent that may still be satisfactory.
Table 3A
<td colspan="2"></td><td> 0</td><td> 15'</td><td> 30'</td><td> 45'</td><td> 60'</td><td> 75'</td><td> 90'</td><td> 105'</td>
<td rowspan="4">Thickness (pm)</td><td>TO</td><td> 0</td><td> 8</td><td> 11</td><td> 13</td><td> 16</td><td> 17</td><td> 23</td><td> 25</td>
<td>B</td><td> 0</td><td> 4</td><td> 6</td><td> 7</td><td> 9</td><td> 10</td><td> 12</td><td> 15</td>
<td>C</td><td> 0</td><td> 7</td><td> 10</td><td> 10</td><td> 13</td><td> 15</td><td> 20</td><td> 25</td>
<td>D</td><td> 0</td><td> 6</td><td> 8</td><td> 10</td><td> 12</td><td> 13</td><td> 19</td><td> 24</td>
<td rowspan="4">Hardness (kgf)</td><td>TO</td><td> 4,00</td><td> 4,04</td><td> 4,10</td><td> 4,51</td><td> 4,55</td><td> 4,77</td><td> 4,40</td><td> 5,45</td>
<td>B</td><td> 4,00</td><td> 4,18</td><td> 5,18</td><td> 4,56</td><td> 6,62</td><td> 6,03</td><td> 6,58</td><td> 7,53</td>
<td>C</td><td> 4,00</td><td> 3,90</td><td> 4,18</td><td> 4,28</td><td> 4,28</td><td> 4,28</td><td> 4,70</td><td> 4,80</td>
<td>D</td><td> 4,00</td><td> 4,08</td><td> 4,40</td><td> 4,39</td><td> 4,36</td><td> 4,75</td><td> 5,58</td><td> 5,29</td>
<td rowspan="4">Disintegration time H2O2 (seconds)</td><td>TO</td><td> 88</td><td> 121</td><td> 118</td><td> 136</td><td> 128</td><td> 162</td><td> 171</td><td> 149</td>
<td>B</td><td> 88</td><td> 146</td><td> 116</td><td> 143</td><td> 142</td><td> 153</td><td> 168</td><td> 153</td>
<td>C</td><td> 88</td><td> 131</td><td> 154</td><td> 188</td><td> 189</td><td> 191</td><td> 239</td><td> 265</td>
<td>D</td><td> 88</td><td> 91</td><td> 125</td><td> 136</td><td> 160</td><td> 160</td><td> 165</td><td> 169</td>
Table 3B
<td>Tablet No.</td><td> 101</td><td> 102</td><td> 103'</td><td> 104</td><td> 105</td><td> 106</td><td> 107</td><td> 108</td><td> 109'</td>
<td>no. of coating</td><td> 13</td><td> 14</td><td> 15</td><td> 16</td><td> 17</td><td> 18</td><td> 19</td><td> 20</td><td> 21</td>
<td>Point in time</td><td> 0</td><td> 0</td><td> 0</td><td> 0</td><td> 0</td><td> 0</td><td> 0</td><td> 0</td><td> 0</td>
<td>Hardness (kgf)</td><td> 5,67</td><td> 5,10</td><td> 4,80</td><td> 6,55</td><td> 5,17</td><td> 4,38</td><td> 5,56</td><td> 4,72</td><td> 4,71</td>
<td>Crumble bility (%)</td><td> 0,00</td><td> 0,00</td><td> 0,37</td><td> 0,13</td><td> 0,00</td><td> 0,24</td><td> 0,13</td><td> 0,00</td><td> 0,01</td>
<td>Disintegration time in H2O</td><td> 00:19</td><td> 00:20</td><td> 00:24</td><td> 00:17</td><td> 00:28</td><td> 00:40</td><td> 00:18</td><td> 00:44</td><td> 00:18</td>
<td>Disintegration time in minutes H2O2</td><td> 01:24</td><td> 01:24</td><td> 03 00</td><td> 01:15</td><td> 03:00</td><td> 02:00</td><td> 01:30</td><td> 01:54</td><td> 01:35</td>
<td>Point in time</td><td>5 d</td><td>5 d</td><td>5 d</td><td>5 d</td><td>5 d</td><td>5 d</td><td>5 d</td><td>5 d</td><td>5 d</td>
<td>Chemical stability</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td>
<td>Hardness (kgf)</td><td> 2,68</td><td> 2,73</td><td> 2,60</td><td> 2,48</td><td> 3,40</td><td> 2,27</td><td> 2,13</td><td> 2,12</td><td> 2,47</td>
<td>Point in time</td><td>13 d</td><td>13 d</td><td>13 d</td><td>13 d</td><td>13 d</td><td>13 d</td><td>13 d</td><td>13 d</td><td>13 d</td>
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<td>Chemical stability</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td><td> 1</td>
<td>Hardness (kgf)</td><td> 2,17</td><td> 2,95</td><td> 2,50</td><td> 2,30</td><td> 3,16</td><td> 2,50</td><td> 2,41</td><td> 1,94</td><td> 2,27</td>
<td colspan="10">(d = days)</td>
The results in Tables 3A and 3B show that coated tablets prepared according to some embodiments of the invention undergo rapid disintegration in the absence of mixing. The disintegration time that was correlated with the type and thickness of the coating was between 01:30 and 04:25 for the placebo tablets having coating thicknesses of up to about 25 µm. It should be emphasized that these durations were obtained in a viscous medium comprising hydrogen peroxide and not in pure water. The basic shade tablets that were coated with various types of coatings obtained disintegration between 01:15 and 03:00 minutes in the same viscous medium. By comparison, basic tone tablets of the same type added to water disintegrated at least two times faster (see tablet # 108) and up to seven times faster (see tablet # 103) with an average of about 4 , 7 times faster for all tested basic shades.
The difference in disintegration time of the various basic shades tested can be derived from the coating type and thickness of the core tablet composition. Interestingly, it was found that ascorbic acid also had a positive impact on disintegration time. A tablet formulation comprising 59% Avicel® PH-102, 24.85% SuperTab® SD-11.2% Croscarmellose sodium Ac-Di-Sol® SD-711 and 1% magnesium stearate. 9.25% N, N-bis (2-hydroxy-ethyl) -p-phenylene-diamine sulfate and 3.9% 4-amino-2-hydroxytoluene, provided uncoated tablet disintegration times of around 04: 30 minutes in H2O2 emulsion. A similar formulation where 3% SuperTab® SD-11 was replaced by 3% ascorbic acid led to tablets disintegrating more rapidly in about 1:30 minutes only. When these tablets were coated with a 5% solution of Brilliant Blue IR Kollicoat®, disintegration times were increased to about 9 minutes for the formulation lacking ascorbic acid, whereas the formulation comprising ascorbic acid provided tablets that were they disintegrated in just three minutes in the H2O2 emulsion without mixing.
The mechanical properties of the tablet as measured immediately after manufacture were satisfactory. The hardness of the basic shade and coated placebo tablets ranged from 3.90 kgf to 7.53 kgf depending on the type of coating and its thickness. The tablets tested had a friableness of at most 0.5%, with the coated placebo tablets having a friableness of less than 0.44% and basic shades having a friableness of between 0.00% and 0.37%. .
Preliminary stability tests of the tablets showed a decrease in hardness under accelerated conditions. The hardness decreased about half of its original value, over the course of 5 days. After this initial decrease, the hardness of the tablets remained approximately stable with average fluctuations of around 2% between day 5 and at least day 13. It should be emphasized that the environmental chamber test conditions are harsher than suggested by the seemingly mild temperature and 65% relative humidity. These accelerated conditions have been reported to be surprisingly more challenging than tests done at 40 ° C and 80% relative humidity. The decrease in hardness observed under accelerated storage conditions led to coated basic shade hardnesses of at least 2 kgf and around 2.5 kgf on average for the basic shades tested. Such values are appropriate for use in dispensing devices such as the dispensing device as described herein.
Importantly, preliminary stability tests of the tablets showed that there was no observable chemical degradation of the color-imparting dyes over the duration of the test.
In further testing, tablet formulations as presented in Table 1E were tested and disintegration was determined in an oxidizing medium (3% hydrogen peroxide, MAG Cosmetics) having a viscosity of about 1.4 cP measured using a Brookfield viscometer around 25 ° C, 50 rpm. For comparison, the disintegration time was also determined in deionized water. The results of these experiments are provided in Table 3C below.
Table 3C
<td>Tone</td><td>No. of tablets in table 1E</td><td>Disintegration time for aqueous hydrogen peroxide coated tablet (seconds)</td><td>Disintegration time for water-coated tablets (seconds)</td><td>Hardness (kgf)</td>
100
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<td>Blue</td><td> 18</td><td> 9</td><td> 10</td><td> 3,7</td>
<td>purple</td><td> 14</td><td> 18</td><td> 6</td><td> 3,8</td>
<td>Red.</td><td> 13</td><td> 10</td><td> 10</td><td> 3,3</td>
<td>Green</td><td> 17</td><td> 4</td><td> 3</td><td> 3,1</td>
<td>natural</td><td> 10</td><td> 15</td><td> 8</td><td> 3,2</td>
<td>rose</td><td> 16</td><td> 3</td><td> 3</td><td> 3,7</td>
<td>Ash</td><td> 15</td><td> 4</td><td> 4</td><td> 3,8</td>
<td>Golden</td><td> 11</td><td> 4</td><td> 4</td><td> 3,4</td>
<td>Orange</td><td> 12</td><td> 9</td><td> 2</td><td> 3,5</td>
Figures 9A and 9B present images of the tablet formulation denoted as tablet 15 in Table 1E, when placed in a 6% (w / w) hydrogen peroxide solution at t = 0 (Figure 9A) and at = 3 seconds (Figure 9B), demonstrating the rapid disintegration time of this exemplary tablet formulation.
In additional sets of experiments, the physical and chemical stability of the coated tablets under various conditions was determined by tests of physical parameters at different time intervals.
The conditions used for the tests were: under an atmosphere of N2; under open air (relative humidity of about 50% at 24 ° C); in oven at a temperature of 40 ° C; in an incubator (relative humidity 65% at 25 ° C) and packed under anhydrous silica gel (anhydrous conditions),
The physical parameters measured were hardness, weight, disintegration time in water and 75% water with 25% H2O2, diameter, friable, appearance and color.
In a representative experiment, the coated tablets are placed in a volumetric flask (i.e., under open air (52% relative humidity, 22.8 ° C)) and the following physical parameters are measured at two week time intervals and one month. Initial results (To) and the results obtained from one month (1 m) are presented in the 3D table below, the results after one month are presented as the change in relation to initial results.
3D table
<td></td><td colspan="2">Hardness</td><td colspan="2">Weight</td><td colspan="2">Disintegration time in H2O (seconds)</td><td colspan="2">Disintegration time in H2O / H2O2 (seconds)</td><td colspan="2">Diameter</td>
<td></td><td>To</td><td>1m</td><td>To</td><td>1m</td><td>To</td><td>1m</td><td>To</td><td>1m</td><td>To</td><td>1m</td>
<td>Blue</td><td> 4,11</td><td> -36 %</td><td> 0,5957</td><td> 2,5 %</td><td> 54</td><td> -48 %</td><td> 205</td><td> -72 %</td><td> 4,59</td><td> 2,8 %</td>
<td>Green</td><td> 4,62</td><td> -48 %</td><td> 0,6192</td><td> 1,88 %</td><td> 19</td><td> -12 %</td><td> 94</td><td> -41 %</td><td> 4,60</td><td> 3,7 %</td>
<td>Red</td><td> 5,00</td><td> -44 %</td><td> 0,6155</td><td> 1,64 %</td><td> 37</td><td> -0,9 %</td><td> 169</td><td> -60 %</td><td> 4,61</td><td> 2,0 %</td>
<td>natural</td><td> 3,8</td><td> -49 %</td><td> 0,6074</td><td> 1,8 %</td><td> 44</td><td> -49 %</td><td> 164</td><td> -56 %</td><td> 4,59</td><td> 3,0 %</td>
<td>purple</td><td> 5,8</td><td> -39 %</td><td> 0,6309</td><td> 2,1 %</td><td> 102</td><td> -50 %</td><td> 181</td><td> -42 %</td><td> 4,52</td><td> 3,2 %</td>
<td>rose</td><td> 4,8</td><td> -47 %</td><td> 0,5817</td><td> 2,3 %</td><td> 16</td><td> -10 %</td><td> 94</td><td> -7,8 %</td><td> 4,67</td><td> 3,2 %</td>
<td>Ash</td><td> 4,9</td><td> -46 %</td><td> 0,588</td><td> 2 %</td><td> 18</td><td> -15 %</td><td> 89</td><td> -69 %</td><td> 4,68</td><td> -</td>
<td>Golden</td><td> 5,8</td><td> -46 %</td><td> 0,6158</td><td> 2,17 %</td><td> 32</td><td> -5,2 %</td><td> 104</td><td> -</td><td> 4,64</td><td> 3,0 %</td>
<td>Orange</td><td> 5,3</td><td> -33 %</td><td> 0,6181</td><td> 1,73 %</td><td> 33</td><td> -2,9 %</td><td> 108</td><td> -19 %</td><td> 4,58</td><td> 2,8 %</td>
As shown in table 3D, the increases in weight and diameter are relatively small.
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These results indicate that little water is absorbed from the atmosphere and therefore suggest good storage stability.
As further shown in Table 3D, the disintegration time is relatively short and decreases with the passage of time.
These results suggest that the tablets disintegrate rapidly in water or in an aqueous H2O2 solution, as it is advantageous, regardless of the storage time.
The lightfastness stability of the tablet coatings was also tested. Overall, 18 coating solutions were prepared and applied to placebo tablets having the following formulation: Avicel® PH-102: 68%; SuperTab® IlSD: 25%; AC-Di-sol® SD711: 3%; magnesium stearate: 1% and ascorbic acid: 3%.
The tablets were coated using coating solutions comprising organic and inorganic pigments.
In a representative stability experiment, several grams of coated tablets are placed in a small container and then placed under the ATLAS instrument. The analysis is done using the SUNTEST CPS + / XLS + Programming Elements Documentation, Version 1.4 Documentation Programming Elements, which simulates direct sunlight (UV light) on the illuminated beads. One hour of illumination corresponds to one month's direct illumination under 3mm thick glass. Since the typical glass thickness in a typical beauty salon is 8mm thick, the tablets are covered with 5mm thick glass to mimic the effect of 8mm thick glass.
Table 3E presents the results as obtained by visual inspection (with the naked eye). Figures 13A-F present images of the coated tablets illuminated during one year of illumination.
Table 3E
<td></td><td>Blue</td><td>Golden</td><td>Orange</td><td>Ash</td><td>Red</td><td>Green</td><td>natural</td>
<td>1 month</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td>
<td>3 months</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td>
<td>6 months</td><td> -</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td><td> ^</td>
<td colspan="8">^ indicates that the coating color of the tablet does not fade (tests are done with the naked eye) -indicates that the color of the tablet coating fades slightly (tests are done with the naked eye)</td>
As shown in Table 3E, all tablet formulations tested exhibited stability for at least 6 months.
The results demonstrate that the compositions and processes disclosed herein result in tablet formulations exhibiting desirable properties.
EXAMPLE 4
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Hair coloring
Tablets prepared as described in Examples 1 and 2 were mixed with appropriate media for the preparation of hair coloring formulas. The formulas were applied on natural yak hair and the color change of the fibers was determined.
In a first series of experiments, the oxidizing and alkaline media were relatively viscous as is customary or the oxidizing media was less viscous and the alkalizing media more viscous, such that the mixtures obtained therefrom had a similar appropriate viscosity. Commonly, up to 150 basic single shade tablets or up to about 300 tablets for blends were added to 60 grams of commercially available 6% H2O2 oxidizing medium having a viscosity of less than 50 cps, as provided by the manufacturer. (MAG Cosmetics) or 60 grams of the previously mentioned diluted Welloxon (2.7% H2O2 and viscosity of 50 cps). The tablets are allowed to spontaneously disintegrate for at most about two minutes for the higher number of tablets. The disintegrated tablets were then hand-brush mixed to homogeneity with the oxidizing medium. 60 grams of a commercially available ammonia based cream (Wella Pure Cream, which has a viscosity of 300 poises or MAG Cosmetics 2% ammonia cream that has a viscosity of more than 300 poises) were added to the premix and mixed in addition to homogeneity. In general, all mixing steps took no more than 3 minutes.
In a second series of experiments, some of the media was prepared using tablets capable of rapidly disintegrating or dissolving to form a desired medium. In a first experiment, the oxidizing medium was made from water and fast disintegration tablets prepared as described herein. 60 tablets of the fast disintegrating oxidant tablet according to tablet # 201 of Table 1C and 60 natural-tone tablets (see tablet # 108) were added to 60 grams of deionized water and allowed to disintegrate as described above. 60 grams of Pure Cream were added and further mixed to homogeneity. In a second experiment, 3 grams of oxidizing tablets according to tablet # 204 were added to 10 grams of water, allowed to disintegrate, and then mixed with 10 grams of Pure Cream. The bleaching effect of this formulation which has a hydrogen peroxide concentration of 2.3% was tested on bundles of naturally pigmented dark human hair and compared to a formulation prepared by mixing 10 grams of 6% H2O2al Welloxon with 10 grams of Pure Cream. In a third experiment, 17 thickening tablets according to tablet # 208 were added to 14 grams of water and allowed to disintegrate. 6 Alkaline tablets according to tablet No. 209 were added to the previous solution and mixed until a creamy formulation was formed.
The final hair preparations, which all had appropriate viscosity regardless of the oxidizing and alkaline media used, were applied generously and thoroughly massaged to completely cover bundles of yak body hair about 7.5 cm long (n. 826401, Kerling International). When the bleaching effect was tested, the light-colored yak hair sample was replaced with pigmented human hair. Unless otherwise indicated, the coloring formulation was applied for 30 minutes and then washed, the hair was completely rinsed in water and allowed to air dry at room temperature.
The coloration of the dry hair was determined visually and reference coordinates were also generated by a hair reader (AvaMouse spectrophotometric measurement, Avantes) that measures the Lab color space and the color spectrum from 380 nm to 750 nm. The measured data were analyzed using Lab Tool Ver. 6.
The results of these experiments are reported in Tables 4A and 4B. For reference, yak hairs treated with the mixture of oxidizing and alkaline media in the absence of tablets have a reference shade corresponding to a Lab spectrum of L: 79.04, a: -0.52 and b: 4.63 . The uncolored and untreated yak hairs showed similar results (L: 77.13, a: -0.09 and b: 7.09).
Table 4A reports the types of tablets tested in this example and each type is assigned for convenience or formulation number (form #). The number of tablets refers to the composition of the tablet core as presented in Table 1B of Example 1 hereinabove for the relevant number of tablets. The number of coatings refers to the tablet coating as given in Table 2 of Example 2 hereinabove for the relevant coating number.
Table 4B reports for each type of tablets used in the preparation of the coloring formulas as described above, first the number of tablets used and below the resulting Lab values (L in the first line, a in the second line and b in the third line of each cell). The Lab values reported represent the average of 5 measurements made on each sample of colored bunches.
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Table 4A
<td>Formulation No.Tone</td><td>1 rose</td><td>two Orange</td><td>3 Red</td><td>4 Golden</td><td>5 purple</td><td>6 Blue</td><td>7 Ash to</td><td>8 natural</td><td>Green</td>
<td>Tablet No.</td><td> 101</td><td> 102</td><td> 103</td><td> 104</td><td> 105</td><td> 106</td><td> 107</td><td> 108</td><td> 09’</td>
<td>Coating No.</td><td> 13</td><td> 14</td><td> 15</td><td> 16</td><td> 17</td><td> 18</td><td> 19</td><td> 20</td><td> 1</td>
Table 4B
<td>No. of rose</td><td> 3</td><td> 6</td><td> 8</td><td> 11</td><td> 14</td><td> 17</td><td> 19</td><td> 22</td>
<td></td><td> 77,71</td><td> 77,40</td><td> 75,80</td><td> 76,72</td><td> 75,05</td><td> 71,78</td><td> 72,79</td><td> 71,54</td>
<td>Pink lab</td><td> 0,95</td><td> 2,54</td><td> 5,52</td><td> 3,57</td><td> 5,85</td><td> 9,72</td><td> 8,38</td><td> 8,92</td>
<td></td><td> 5,95</td><td> 7,38</td><td> 10,73</td><td> 8,15</td><td> 10,79</td><td> 14,78</td><td> 13,85</td><td> 14,27</td>
<td>Orange No.</td><td> 13</td><td> 26</td><td> 40</td><td> 53</td><td> 66</td><td> 79</td><td> 93</td><td> 106</td>
<td></td><td> 61,27</td><td> 55,02</td><td> 50,16</td><td> 49,82</td><td> 47,50</td><td> 47,80</td><td> 46,33</td><td> 44,53</td>
<td>Orange lab</td><td> 24,88</td><td> 33,30</td><td> 37,68</td><td> 39,07</td><td> 40,60</td><td> 40,76</td><td> 42,48</td><td> 42,21</td>
<td></td><td> 50,74</td><td> 55,90</td><td> 54,54</td><td> 54,98</td><td> 52,07</td><td> 52,20</td><td> 50,06</td><td> 48,01</td>
<td>Red No.</td><td> 18</td><td> 37</td><td> 55</td><td> 74</td><td> 92</td><td> 111</td><td> 129</td><td> 148</td>
<td></td><td> 52,69</td><td> 48,21</td><td> 47,79</td><td> 47,11</td><td> 45,00</td><td> 41,23</td><td> 43,80</td><td> 38,42</td>
<td>Red lab</td><td> 36,02</td><td> 39,58</td><td> 41,63</td><td> 41,10</td><td> 41,69</td><td> 43,14</td><td> 42,78</td><td> 44,83</td>
<td></td><td> 30,13</td><td> 33,29</td><td> 35,21</td><td> 32,87</td><td> 35,36</td><td> 35,53</td><td> 34,87</td><td> 35,24</td>
<td>No. of dorado</td><td> 5</td><td> 10</td><td> 14</td><td> 19</td><td> 24</td><td> 29</td><td> 33</td><td> 38</td>
<td></td><td> 74,89</td><td> 72,38</td><td> 69,71</td><td> 67,47</td><td> 65,66</td><td> 63,94</td><td> 64,30</td><td> 61,36</td>
<td>Golden lab</td><td> 5,64</td><td> 9,24</td><td> 14,35</td><td> 17,72</td><td> 19,23</td><td> 19,83</td><td> 20,70</td><td> 24,31</td>
<td></td><td> 24,37</td><td> 31,14</td><td> 38,56</td><td> 43,36</td><td> 46,34</td><td> 45,79</td><td> 46,60</td><td> 50,96</td>
<td>No. of violet</td><td> 10</td><td> 21</td><td> 31</td><td> 41</td><td> 51</td><td> 62</td><td> 72</td><td> 82</td>
<td>Violet Lab</td><td> 44,95</td><td> 35,99</td><td> 28,21</td><td> 30,33</td><td> 25,96</td><td> 24,68</td><td> 21,89</td><td> 22,66</td>
<td></td><td> 7,45</td><td> 10,63</td><td> 12,76</td><td> 11,45</td><td> 12,56</td><td> 11,12</td><td> 11,96</td><td> 11,91</td>
<td></td><td> -18,96</td><td> -23,09</td><td> -23,75</td><td> -23,34</td><td> -24,13</td><td> -22,00</td><td> 22,64</td><td> 22,21</td>
<td>Blue No.</td><td> 12</td><td> 23</td><td> 35</td><td> 46</td><td> 58</td><td> 69</td><td> 81</td><td> 92</td>
<td>Blue lab</td><td> 44,23</td><td> 34,25</td><td> 30,89</td><td> 27,35</td><td> 25,71</td><td> 24,41</td><td> 25,96</td><td> 22,42</td>
<td></td><td> -4,90</td><td> -1,80</td><td> 0,19</td><td> 1,38</td><td> 2,33</td><td> 1,53</td><td> 1,40</td><td> 3,27</td>
<td></td><td> -23,26</td><td> -24,86</td><td> -25,19</td><td> -24,44</td><td> -24,94</td><td> -21,97</td><td> 22,58</td><td> 22,50</td>
<td>Ash No.</td><td> 5</td><td> 9</td><td> 14</td><td> 18</td><td> 23</td><td> 28</td><td> 32</td><td> 37</td>
<td>Ash lab</td><td> 75,19</td><td> 68,15</td><td> 66,36</td><td> 62,97</td><td> 58,23</td><td> 56,38</td><td> 52,62</td><td> 50,60</td>
<td></td><td> -0,49</td><td> -0,17</td><td> -1,04</td><td> -1,17</td><td> -0,84</td><td> -0,73</td><td> -0,46</td><td> 0,21</td>
<td></td><td> 1,30</td><td> -3,08</td><td> -5,24</td><td> -7,66</td><td> -10,01</td><td> -10,84</td><td> 11,49</td><td> 13,52</td>
<td>Natural No.</td><td> 9</td><td> 28</td><td> 37</td><td> 46</td><td> 65</td><td> 74</td><td> 83</td><td> 102</td>
<td></td><td> 58,29</td><td> 36,90</td><td> 35,53</td><td> 35,45</td><td> 29,91</td><td> 28,45</td><td> 27,20</td><td> 22,82</td>
<td>Natural lab</td><td> 2,95</td><td> 4,45</td><td> 4,83</td><td> 4,54</td><td> 4,61</td><td> 4,38</td><td> 4,38</td><td> 3,88</td>
104
ES 2 823 977 T3
<td></td><td> 11,31</td><td> 13,28</td><td> 13,92</td><td> 15,48</td><td> 13,32</td><td> 12,11</td><td> 10,98</td><td> 9,25</td>
<td>No. of green</td><td> 9</td><td> 18</td><td> 28</td><td> 37</td><td> 46</td><td> 55</td><td> 65</td><td> 74</td>
<td></td><td> 55,49</td><td> 46,15</td><td> 40,01</td><td> 37,05</td><td> 32,77</td><td> 31,17</td><td> 29,35</td><td> 27,79</td>
<td>Green lab</td><td> -0,18</td><td> -0,15</td><td> 0,14</td><td> -0,39</td><td> -0,23</td><td> 0,16</td><td> -0,01</td><td> 0,07</td>
<td></td><td> 10,50</td><td> 11,79</td><td> 11,08</td><td> 12,70</td><td> 11,01</td><td> 10,94</td><td> 9,29</td><td> 8,90</td>
The results presented in Table 4B show that the lighter component of the color presentation, L decreases with the increased number of tablets. Chromaticity components a and b, also called opponent color axes, were affected differently by the increased number of tablets depending on the basic shades being tested. For information, component a represents approximately the advance of color between red / magenta (positive) and green (negative) colors, while component b is an indicator of the evolution from yellow (positive) to blue (negative) colors. ) the relationships between the Lab values at different points tested need not be linear, as this method of color presentation is intended to mimic the non-linear response of the eye. Visual determination of dry colored hair bundles showed good coloring, which progressed with increasing number of tablets from lighter to darker shades of each basic shade. The colored bunches corresponding to the aforementioned experiments are illustrated in Figures 15A-15I. The number of tablets used in the final formula is indicated at the base of each yak hair bundle and the tone and formulation number is indicated for each panel.
In a separate set of experiments, a preparation equivalent to Formula 9 was prepared by thickening the individual ingredients and incorporating them into the media in powder form rather than tablet form. The staining was carried out and monitored as previously described. The results were similar to those obtained for the corresponding tablet formulation, indicating that tablet formulations as described herein do not affect the coloring performance of the color-imparting agents encompassed herein.
Mixes of basic shades of different types also resulted in pleasant coloring. The result is a combination of red (formulation # 3) and violet (formulation # 5), when applied to yak hair, in a darker purple shade, while the combination of blue (formulation # 6) and natural (formulation # 8) resulted in a darker blue hue. Mixtures of up to five basic shades were prepared and their Lab values were measured. A first mix containing 175 natural tablets, 29 orange tablets, 18 gold tablets, 10 ash tablets and 6 violet tablets (formulation # 10) prepared in a final volume of 120 grams of coloring formula led to a nutty coloring with L: 19.01, A: 7.38 and b: 11.37. A second mixture comprising 130 red tablets, 115 natural tablets, 43 orange tablets, 10 gold tablets and 6 violet tablets (formulation # 11) led to a warm reddish brown color with L: 19.53, a: 17.53 b: 9.68. A third blend comprising 105 natural tablets, 100 red tablets, 11 violet tablets and 7 orange tablets (formulation # 12) led to a mahogany coloration with L: 18.39, a: 15.93 and b : 6.09.
The media tablets allowed the preparation of formulations that allow coloring or discoloration as desired. The coloring formulation prepared with natural basic shade and oxidizing agents in fast disintegrating tablet forms produced the expected natural walnut coloring with Lab values of L: 24.81, a: 5.23 and b: 11.74. These results are comparable to the Lab values obtained with 65 tablets of the same basic shade when the oxidizing agent was distributed in a commercially available hydrogen peroxide emulsion.
The prepared bleaching tablet formulation lightened the shade of the sample human hair in a manner comparable to the control formulation made from commercially available alkaline and oxidizing media. Untreated human hair reference Lab values L: 20.84, a: 3.49 and b: 4.51, while hair treated with a corresponding tablet formulation showed Lab values of L: 23.48, a : 6.97 and b: 8.54 and hair treated with a commercially available formula showed Lab values of L: 21.48, a: 5.84 and b: 7.65. The experiment conducted with thickening tablets which were first allowed to disintegrate before the alkaline tablets were added demonstrated that the viscosity of the media could be controlled by adding the tablets as described herein.
These results demonstrate that basic shades and media tablets prepared according to some embodiments of the invention can be used for the preparation of coloring formulas. The coloring formulas, whether comprising an increased number of tablets of a given shade or mixtures of basic shades, effectively modified the color of the fibers being tested. These results further demonstrate that rapid disintegration tablets as described herein, when used in combination
105
ES 2 823 977 T3 with water, can replace the traditional means used in coloring procedures.
Additional experiments were carried out to determine the effect of hair type on hair coloring.
In a series of experiments, single-tone colorations were performed on natural human laboratory hair of different types: blond Caucasian hair, dark blond Caucasian hair, and dark Caucasian hair. Each shade was tested with three different amounts of tablets. For example, the natural tone was applied using 1 , 34 or 67 tablets in 60 ml of alkaline medium and 60 ml of oxidizing medium and the green tone was applied using 1, 101 or 200 tablets in 60 ml of alkaline medium and 60 ml of oxidizing medium.
In another series of experiments, all possible combinations of two shades in a wide range of proportions were applied to different hair types, ranging from lighter Caucasian hair to darker Asian hair, as well as yak hair. Exemplary combinations included one orange-hued tablet with 100 purple-hued tablets; 100 orange tablets with 1 purple tablet and 100 orange tablets with 100 purple tablets. Each of the aforementioned combinations of tablets was added to 60 ml of medium and 60 ml of hydrogen peroxide solution. The peroxide solution and 2% ammonia cream medium were obtained from MAG Cosmetics. The resulting color obtained for each hair type exhibited an impact of natural pigmentation and coloring of the coloring agent (that is, the number of tablets used).
In all these experiments, tablets denoted with number 3 (orange), number 8 (green) and number 5 (purple) in Table 1D, were used.
Figure 16A shows the hair color obtained with three concentrations of green tone, when applied to natural dark blonde Caucasian hair.
As shown in Figure 16B, after the application of a combination of orange and violet tones, the orange tone had little impact when applied in low amounts (sample 1), the violet tone had little impact when applied in low amounts. amounts (sample 2) and both shades had a considerable impact when applied in similar amounts (sample 3).
As shown in Figure 17, human natural red hair was colored copper-red using a commercially available Koleston Perfect tube (copper red shade), mixed 1: 1 with Welloxon 6% hydrogen peroxide cream. After coloring with Koleston shade, further application of purple shade tablets resulted in a burgundy color.
These results indicate that the color obtained using exemplary tablets is a function of the number of tablets used and the initial hair color (which depends on the natural hair pigmentation and previous coloring, if any).
EXAMPLE 5
Tablet drying
A process for drying tablets was developed in order to increase stability and shelf life.
In a typical procedure, coated tablets having the formulations presented in Table 1E, coated with a PVA coating purchased from Colorcon Opadry 200, were placed in a vacuum oven for 20 hours. Moisture content was measured using a Sartorius MA 150 Moisture Analyzer by manually grinding 1 gram of tablets (from each sample) and measuring the weight change at 120 ° C at a pressure of 3 kPa (30 mbar) for 1 hour.
As shown in Table 5A below, the water content of the tablets of all basic shades was reduced to less than 3% and even less than 1%.
Table 5A
<td>Tone</td><td>Water content after drying process (percent by weight)</td>
<td>Green</td><td> 0,9</td>
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ES 2 823 977 T3
<td>Orange</td><td> 1,8</td>
<td>Golden</td><td> 1,9</td>
<td>rose</td><td> 2,1</td>
<td>Ash</td><td> 2,0</td>
<td>Blue</td><td> 2,5</td>
<td>natural</td><td> 2,3</td>
<td>Red</td><td> 1,8</td>
<td>purple</td><td> 2,6</td>
These results indicate that the water content of tablets according to some embodiments of the invention can be reduced to low levels (eg, less than 3%), thereby improving the stability of the tablet, despite the presence of ingredients. hygroscopic.
EXAMPLE 6
Microbiological stability of tablets
In order to test the stability of exemplary tablets towards microbiological contamination, tablet samples were stored under relatively anhydrous conditions (2% relative humidity, 25 ° C) for a period of time ranging from 3 to 24 weeks. All tablets had a formulation as presented in Table 1E. In each sample, both the initial and final concentration of colony forming units (CFU) were less than 10 CFU / gram.
These results indicate that the tablets described herein exhibit microbiological stability, particularly when stored under relatively anhydrous conditions.
EXAMPLE 7
HPLC Analysis of Coloring Agents
In view of the repeated use of the exemplary coloring agents described in the examples herein, an analytically sensitive method for detecting amounts of coloring agent was developed using HPLC (high performance liquid chromatography). Such a method may be useful, for example, to accurately quantify the chemical stability of tablets containing coloring agents (eg, tablets described herein).
A Sepax® chromatographic column (GP C718 4.6X250 mm 5u; 120A) with phosphate buffer solution (50 Mm, pH 3.0) was used as mobile phase. Gradient flow was as described in Table 7A.
Table 8A
<td>% B = Acetonitrile</td><td>% A = Phosphate buffer solution</td><td>Time (minutes)</td>
<td> 0</td><td> 100</td><td> 0</td>
<td> 0</td><td> 100</td><td> 3</td>
<td> 50</td><td> 50</td><td> 30</td>
<td> 50</td><td> 50</td><td> 33</td>
<td> 0</td><td> 100</td><td> 33,1</td>
<td> 0</td><td> 100</td><td> 40</td>
A LaChrom (Hitachi) HPLC system was used with a L-7100 solvent pump, L-7200 audiosampler, L-7300 column oven, and DA-L7455 photodiode array detector. The flow rate was 1.0 ml / minute; the injection volume was 10 µl; detection between 200-400 nm.
The samples were dissolved (usually 1 mg / ml) in water or a water / acetonitrile solution in a 107 flask.
ES 2 823 977 T3 100 ml volumetric. The flask was shaken to fully dissolve the coloring agent and an injection bottle was prepared using an appropriate filter (eg, a PTFE filter).
The retention time of exemplary agents used in formulations described herein is presented in Table 8B below and a representative HPLC spectrum is shown in Figure 14.
Table 7B
<td>Retention time (minutes)</td><td>Compound</td>
<td> 4,13</td><td>Toluene-2,5-diaminosulfate</td>
<td> 3,04</td><td>1-Hydroxyethyl-4,5-diaminopyrazole sulfate</td>
<td> 10,50</td><td>N, N-bis (2-hydroxyethyl) -p-phenylenediamine sulfate)</td>
<td> 6,26</td><td>4-amino-3-methylphenol</td>
<td> 4,02</td><td>1-hydroxy-4-aminobenzene</td>
<td> 13,33</td><td>5-amino-2-methylphenol</td>
<td> 6,72</td><td>2,4-diaminophenoxy-ethanol</td>
<td> 6,69</td><td>m-aminophenol</td>
<td> 15,20</td><td>Resorcinol</td>
<td> 13,76</td><td>Hydroxyethyl-3,4-methylene dioxyaniline HCl</td>
<td> 25,84</td><td>2-amino-6-chloro-4-nitrophenol</td>
<td> 20,00</td><td>HC Red # 10</td>
<td> 17,30</td><td>HC Red # 11</td>
<td> 22,34</td><td>HC Yellow # 13</td>
<td> -</td><td>2,6-diamino-3-pyridin-3-yl-azo-pyridine</td>
<td> 29,52</td><td>HC Blue # 15</td>
<td> 4,85</td><td>Ascorbic acid</td>
These results indicate that quantities of exemplary agents can be accurately quantitatively determined.
EXAMPLE 8
Exemplary alkaline and oxidizing media grams of a commercially available 1% ammonia cream (MAG Cosmetics), having a viscosity of more than 300 cP, were diluted with water at a weight ratio of 1: 2 (cream: water) to slowly add water to cream during continuous hand mixing. 30 grams of an ammonia-based alkalizing medium in the form of a pourable cream were obtained.
108
ES 2 823 977 T 3 grams of 6% hydrogen peroxide solution (containing 1% EDTA, pH 2.8 adjusted with phosphoric acid) were then added globally to the pourable cream, alkalizing medium and mixed vigorously by hand. The result was a very dilute cream with the consistency of lotion, which thickened slightly over time but remained fully pourable.
In a further experiment, 0.9 grams of Novethix ™ polymer L-10 (Lubrizol, 30% by weight suspension of polymer in aqueous solution) and acrylate / behenethio-25 methacrylate copolymer were added to 29.1 grams of the above-mentioned 6% hydrogen peroxide solution (pH 2.8), to obtain 30 grams of oxidizing medium comprising 3% by weight of the thickening agent polymer. This thickening agent is an anionic polymer that has little effect on viscosity under acidic conditions, when the polymer is in the protonated nonionic state. Thus, the addition of the thickening agent did not substantially change the consistency of the acidic oxidizing medium. This oxidizing medium with thickening agent was added overall to 30 grams of the alkalizing medium described above and mixed vigorously for 30 seconds. The mixture immediately thickened and after about 2 minutes turned into a thick cream.
EXAMPLE 9
Exemplary distributor device
A device capable of dispensing measured amounts of tablets contained in separate containers was constructed as schematically illustrated in Figure 2, with containers as shown in Figure 6 and dispensing means as partially shown in Figure 8. The device had overall dimensions 345mm (width) * 345mm (depth) * 525mm (height, including containers). The device had 16 approximately cylindrical containers made of polyethylene terephthalate (PET) manufactured by blow molding. The diameter of the container was around 60 mm and its walls were around 200 mm high. Each container was equipped with a shutter mechanism as shown in Figure 43, facilitating quick and convenient replacement of a container while preventing the tablets from spilling. The two partial spherical covers that make up the shutter mechanism were made of plastic, manufactured by injection molding, the serrated path was made of plastic, manufactured by injection molding, was attached to the outside of the container. Above the tablet outlets of each sprocket, a steel wire was mounted, preventing the tablets from being accidentally distributed out directly (ie, not via the sprocket mechanism).
The stepper motors were placed under their respective containers under the stainless steel platform in a manner that allowed free flow of the distributed tablets to a four sloped wall plastic funnel that was prepared by plastic rapid prototyping. A shutter mechanism at the outlet of the funnel provided control of the actual movement in which the tablets are delivered from the device. The shutter mechanism consisted of a rubber ball that, unless pulled up by the electromechanical actuator, blocked the outlet of the funnel. Two additional optical detectors were positioned around the position of the receiving container, which is intended to provide indication of its presence in order to prevent tablets from being delivered from the device as long as no container is in place. The stepper motors (42 permanent magnet stepper motor, which has a 15 ° stage angle and a holding torque of 800 g.cm) allowed delivery at a rate of up to 2,880 tablets per minute (using a sprocket with 24 tooth spaces at a maximum rotation of 120 rpm). In general, repeatability tests were carried out up to 80 rpm using spheroidal placebo tablets having an average diameter of about 5 mm.
The device comprises two optical sensors (Everlight Photodetector Transistor, PT204-6B) for each outlet of the container. The stepper motors and their corresponding photodiodes were mounted on a single PCB formed to match the side arrangement of the vessels. An additional PCB that contained all the electronic components of the control also as means of Connectivity to a personal computer installed inside the distributor. The additional PCB was used to control a touch screen LCD that serves as a user interface configured to allow manual entry of the desired number of tablets from each specific container. Numerous experiments were carried out successfully. Repeatability tests, where the number of tablets distributed was each time confirmed by manual counting, establishing that the device was accurate and feasible.
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Contents65
56 sheets
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Numbers
- Publication
- 2823977
- Publication, DOCDB
- 2823977
- Publication, EPODOC
- ES2823977T
- Application
- 12716622
- Application, DOCDB
- 12716622
- Application, EPODOC
- ES20120716622T
Titles2
- Spanish
- Sistemas para coloración personalizada
- English
- Systems for custom coloring
Classification
- CPC, 36
- A45D44/005
- A61K8/731
- A61K8/732
- A61Q5/10
- G01N21/25
- A61K8/73
- A61K8/0216
- A61K8/8176
- G01N33/4833
- A45D2200/058
- A61K2800/87
- A45D19/0066
- B01F21/20
- B01F33/841
- B01F33/8442
- A45D19/02
- A45D44/02
- A45D2044/007
- G16H20/70
- Y02A90/10
- B01F35/714
- G01N21/00
- A61K8/81
- A61K8/02
- A61Q5/06
- A61K8/347
- A61K8/40
- A61K8/415
- A61K8/463
- A61K8/4926
- A61K8/494
- A61K8/817
- A61K2800/4324
- A61K2800/48
- G01N21/4738
- G01N2201/06146
- IPC, 17
- A61K8 34
- A61K8 49
- A61K8 46
- A45D19 02
- A45D44 02
- A61K8 73
- A61Q5 10
- A45D44 00
- A61K8 40
- A61K8 41
- A61K8 81
- A61K8 02
- B01F13 10
- B01F15 02
- B01F1 00
- G01N33 483
- G01N21 47