Methods of making compositions comprising films

[0001] The present application relates to methods for preparing compositions containing films.

BACKGROUND OF THE INVENTION [0002] Films containing consumable or active materials are useful in a wide variety of applications, including oral care, personal hygiene, household and cleaning products. Such films are typically found in the carrier or product of the product. During use, these films generally degrade by chemical or physical rupture, whereby active or useable material is released into the surrounding environment. In this way, the films give the opportunity to locally release a high concentration of active materials near the target surface.

[0003] Conventional methods for forming such materials involve the introduction of usable or active materials into the film in the manufacturing process. The film is then often cut into flakes or parts, which are introduced into the product carrier and dispersed in it. However, there is a possibility that the active material in the film may become unstable during storage due to potential migration from the film to the carrier and / or the negative interaction of the active material contained in the film with incompatible carrier components. In addition, the additional step of adding active material to the film in the production process increases production costs.

[0004] Alternative and improved methods of making films containing such active materials for a wide variety of consumer products are therefore desirable.

It is also desirable to develop compositions that are stable during storage.

[0005] US-A-2002/131990 discloses pullulan-free edible film compositions and methods for their preparation. WO-A-2005/079750 discloses films for use as dosage forms.

BRIEF SUMMARY OF THE INVENTION [0006] The present invention provides a method according to claim 1, for the preparation of a composition for oral care, personal hygiene, cleaning and / or household use. The method includes immersing the film in a medium containing the active ingredient, the film essentially free of this active ingredient; transferring at least a portion of this active ingredient from the medium to the film based on a concentration gradient of the active ingredient between the medium and the film, wherein the transfer occurs until the film contains an effective amount of the transferred active ingredient, so that the film can be used in at least one of compositions for oral care, personal hygiene, for cleaning and / or use in the household; and preparing this composition by incorporating a film containing the transferred active ingredient into the carrier film, wherein the dissolution rate of the carrier film is higher than the dissolution rate of the film containing the active ingredient and wherein the film containing the transferred active ingredient is stable during storage of the composition.

[0007] Advantageous features are defined in the dependent claims.

DETAILED DESCRIPTION OF THE INVENTION [0008] In the present description, ranges are used as a transcript for describing a single and each value falling within a given range. Any value within the range can be selected as the end value of that range. Unless otherwise specified, in this specification all references to the concentration of the ingredients are given by weight.

[0009] In various embodiments, the invention provides methods for making a film that includes the active ingredient. Specifically, embodiments of the invention relate to methods for incorporating the active ingredient into a film.

[0010] Films containing active ingredients are useful in many different types of compositions, especially in consumer products such as oral care, personal hygiene, cleaning and / or household use products. Such compositions generally comprise a carrier into which the film is inserted and in which it is arranged. In general, the active ingredients are incorporated into the film along with other precursors during the production of this film, i.e. during solvent immersion molding, extrusion, blow molding and the like. Then, the film containing the active ingredient is added to the composition carrier.

[0011] However, this method of incorporating the active ingredient into a film can be quite expensive. It generally requires an additional process step during manufacture, and may also result in loss of process efficiency. In addition, it can limit the process conditions during film production required to protect the active ingredient from deactivation or degradation by factors such as heat, pressure, excessive physical strength, corrosive solvents or care products. When the active ingredient is incorporated into the composition carrier, there is an additional risk of film instability in this carrier. For example, from time to time the active ingredient diffuses from the film into the carrier, which reduces the localized concentration of the active ingredient in this film and reduces the effectiveness of the composition.

[0012] Improved methods have been introduced in various embodiments of the present invention. In a preferred method, the film is immersed in a medium containing the active ingredient, the film being substantially free of the active ingredient, and wherein the film is such that the active ingredient can conveniently be incorporated therein. The term "substantially free of" as used herein means that the active ingredient is not present in the film to such an extent that it is present in a degree of efficacy and / or undetectable. At least a portion of the active ingredient present in the medium is then transferred to the film based on a concentration gradient of the active ingredient between the medium and the film.

[0013] The term "transfer" as used herein refers to the displacement or transport of an active ingredient from a medium to a film. The term includes both passive and active movement of the active ingredient molecules into the film. Passive transfer generally does not require an external factor (e.g. mechanical force, chemical and / or thermal energy) to achieve movement of the active ingredient. In general, passive transfer involves mass transport phenomena, including diffusion, in which the active ingredient molecules are physically transported through a concentration gradient until reaching thermodynamic equilibrium. Passive transfer can also include electrochemical interaction, absorption, adsorption and / or wick movement of the active ingredient into the film, where no external agent is required to achieve sufficient movement of the active ingredient into the film. Active transport refers to the use of an external force or medium, such as temperature, pressure, electrical and / or mechanical force to achieve the displacement of the active ingredient from the medium to the film. For example, the use of an external force or factor may support the displacement of active ingredient molecules through an electric gradient or physical transport barrier.

[0014] In some embodiments, a method is provided for making compositions for oral care, personal hygiene, cleaning and / or household use. This method involves immersing the film in a medium containing the active ingredient. This film is essentially free of active ingredient and is of such a nature that the active ingredient can be transferred into it. In some implementations, the film is porous. At least a portion of the active ingredient present in the medium is transferred to the film by a concentration gradient of the active ingredient between the medium and the film. This transfer occurs until the film contains an effective amount of the transferred active ingredient, so that the film is suitable for use in at least one composition for oral care, personal hygiene, cleaning and / or household use. This composition is prepared by introducing a film containing the transferred active ingredient into the carrier, wherein the film containing this transferred active ingredient is stable during storage of the composition.

[0015] An "effective" amount of an active ingredient is an amount that contributes to and / or has a detectable effect for the intended purpose and / or use. Preferably, this effective amount is sufficient to exert the desired therapeutic, cleansing and / or prophylactic effect on the target (e.g., human or lower animal, household surface or the like) in which or in which the composition comprising this film is used. Preferably, the active ingredient does not exert undesirable undesirable side effects (such as toxicity, irritation, allergic reactions) disproportionate to a rational risk / benefit ratio. The specific effective amount of active ingredient will vary and will depend on factors such as the condition or subject being treated, physical condition, type of parallel therapy (if conducted), specific active ingredient used, specific dosage form, carrier used, and desired dosage regimen.

[0016] Thus, the choice of active ingredient depends on the applications in which these compositions will be used, i.e. on their intended purpose. Thus, the term "active ingredient" as used herein is a material having the desired utility in the composition. In various implementations, such utilities may be cleaning, protection, treatment, cosmetic, aesthetic, decorative and sensory effects, or combinations thereof. As stated above, the compositions of the invention can be used on a wide variety of target surfaces, including industrial surfaces, in the household, on the somatic surfaces of the human and animal body, especially on oral, skin and calloused surfaces. Non-limiting examples of target surfaces include oral surfaces such as dental enamel; skin surfaces such as skin; horny tissue surfaces such as nails and hair; Household surfaces such as metal items, fastened items, fibers, fabrics, tableware, home furnishings, tiles, floors, ceramics, metal products and the like. Active ingredients include those selected to be separately maintained in the carrier and delivered and released independently through the film, and may include compounds or components that are treated as carrier components and vice versa.

[0017] Films containing the active material may be provided, for example, in an oral care composition, which may be in the form of a dentifrice (including toothpastes, tooth gels, mouthwashes, tooth powders and preventive pastes) ), sweets (including gums, balls and chewing gums), foil, paint-on varnishes, professional polishing formulation or any other form known to those skilled in the art. These films can also be used in personal care compositions such as soaps, bath gels, body washers, exfoliating scrubs, shampoos, lotions, sun creams, self-tanning products, antiperspirants and deodorants, nail care products and the like. Similarly, these films can also be used in household cleaning products and / or compositions, including e.g. powders, pastes, dishwashing liquids and detergents for automatic dishwashers, detergents and fabric softeners, and hard surface cleaners.

[0018] The following description of the active ingredients is merely exemplary and should not be considered as limiting the range of active ingredients that can be incorporated into films by the methods of the invention, as all suitable active ingredients known to those skilled in the art for these various types of compositions are contemplated. It is understood that while the general properties of each of the above categories of active ingredients may differ in activity, there may be some common characteristics and any selected material may serve a variety of purposes within two or more categories and may be suitable for use in various types of compositions.

[0019] Non-limiting examples of oral care active ingredients used in oral care compositions include, for example, teeth whitening agents, antibacterial agents, anti-caries agents, tartar agents, anti-plaque agents, anti-adhesive agents, desensitizing agents, anti-inflammatory agents , deodorising agents, fragrances, coloring agents, anti-aging agents, salivary stimulants, periodontal active agents, tonics, moisturizers, skin irritants, natural extracts and essential oils, nutrients, enzymes, proteins, amino acids, vitamins, painkillers, antibiotics and mixtures thereof. Exemplary active ingredients among those that are useful in the present invention are disclosed in US Patent Nos. US 4,894,220 (Nabi et al.), US 5,288,480 and US 5,776,435 (both belonging to Gaffar et al. .), US 5,681,548 (Esposito et al.)., US 5,912,274 and US 5,723,500 both belonging to Stringer et al.), US 6,229,933 (Durga et al.) And US 6,685,921 (Lawror ) and United States Patent Application Publication No. 2003/0206874 (Doyle) et al.). In addition, mixtures of active ingredients for oral care are intended to be used in the present invention, even within the same classification.

[0020] Examples of suitable orally active ingredients include whitening agents for oral surfaces such as teeth. In various embodiments, the film compositions of the invention contain one or more bleaching agents in the film. As described below, "whitening agent" is a material that effectively whitens the surface of the hard tissue in the mouth (eg, enamel or other tooth surfaces) on which it is applied. In one embodiment of the invention, the whitening agent comprises a peroxide compound. As used herein, "peroxide compound" is an oxidizing compound containing a divalent oxygen-oxygen group.

[0021] In some embodiments, the active ingredient comprises a peroxide compound, which is preferably present in the entire oral care composition in any amount sufficient to produce a detectable whitening effect. "Concentration equivalent to hydrogen peroxide concentration" for a given peroxide compound refers to the amount of compound with an active peroxide that produces hydrogen peroxide ion or an organic peroxide ion in an amount equivalent to the amount of hydrogen peroxide ion supplied by pure hydrogen peroxide under the same conditions.

[0022] Preferably, the peroxide compounds are present in the oral care compositions in an amount corresponding to a concentration equivalent to the concentration of hydrogen peroxide in this oral care composition of from about 1 to about 15%; optionally from about 1 to about 10%; optionally from about 3 to about 10% by weight of this composition. In some preferred embodiments, the concentration equivalent to the hydrogen peroxide concentration is from about 2% to about 8%; in some implementations it is about 6%.

[0023] A suitable peroxide compound (s) may be any peroxide-based whitening agent that releases a hydrogen peroxide ion or an organic peroxide ion. Peroxide compounds include peroxides and hydroperoxides such as hydrogen peroxide, alkali metal and alkaline earth metal peroxides, organic peroxide compounds, peroxy acids, and pharmaceutically acceptable salts and mixtures thereof.

[0024] In some embodiments of the invention, the whitening agent is an inorganic hydrogen peroxide generating compound, such as, for example, salts of peroxosulfate, peroxodisulfate, percarbonate, peroxophosphate, perborate and peroxosilicate with an alkali metal and alkaline earth metal, such as, for example, sodium peroxosulfate, sodium peroxodisulfate, sodium percarbonate, sodium peroxophosphate, sodium perborate, sodium peroxosilicate, potassium peroxosulphate, potassium peroxodisulfate, potassium percarbonate, potassium peroxophosphate, potassium perborate, potassium peroxosilicate, lithium peroxosulphate, lithium peroxocarbonate, lithium peroxophosphate, lithium perborate, lithium peroxosilicate, calcium peroxosulphate, calcium peroxosulphate, calcium peroxosulphate, calcium peroxosulphate , barium peroxodisulfate, barium percarbonate, barium peroxophosphate, barium perborate, barium peroxosilicate, magnesium peroxosulfate, magnesium peroxodisulfate, magnesium percarbonate, magnesium peroxophosphate, magnesium perborate, magnesium perosilicate, as well as sodium peroxide, potassium peroxide, lithium peroxide, calcium peroxide, barium peroxide and magnesium peroxide, and combinations of the above compounds.

[0025] In some embodiments, the whitening agent contains organic peroxy compounds, including carbamide peroxide (also known as hydrogen peroxide and urea complex), glycerol hydroperoxide, alkyl hydroperoxides, dialkyl peroxides, alkylperoxy acids, peroxy esters, diacyl peroxides, benzoyl peroxide and monoperoxyphthalate and mixtures thereof. Peroxy acids and their salts include organic peroxy acids such as alkylperoxy acids and monoperoxyphthalate and mixtures thereof as well as salts of inorganic peroxy acids such as salts of peroxosulfate, peroxodisulfate, percarbonate, peroxophosphate, perborate and peroxosilicate with alkali metals and earth metals alkali, such as lithium, potassium, sodium, magnesium, calcium, and barium, and mixtures thereof. In various embodiments, the peroxide compound is hydrogen peroxide, a hydrogen peroxide complex with urea, sodium percarbonate, and mixtures thereof.

[0026] Peroxide releasing compounds particularly useful as the active ingredients of whitening agents in the oral care compositions of the invention include peroxide containing compounds such as a hydrogen peroxide complex with urea, sodium percarbonate, sodium perborate and polyvinylpyrrolidoneH2O2 complexes (hereinafter referred to as "PVP- H2O2 "). PVP or polyvinylpyrrolidone is known as poly-N-vinyl-poly-2-pyrrolidone. Complexes of both linear and cross-linked PVPH2O2 are known in the art and are disclosed in US Patent Publication Nos. 3,376.110 and 3,480,557 (both belonging to Shiraeff) and in US 5,122,370 (Merianos et al. ). PVP-H2O2 is stable in anhydrous environment. When in contact with an environment with a large amount of water, such as that prevails in the mouth, PVP-H2O2 will dissociate into individual compounds (PVP polymer and H2O2). In one embodiment, the PVP-H2O2 complex contains about 80% polyvinylpyrrolidone and 20% H2O2. The concentration of PVP in the PVPH2O2 complex is independent of the potential concentrations of PVP in cases where PVP is used as the polymer to form the film.

[0027] In various embodiments, the whitening agent comprises a peroxide compound, such as hydrogen peroxide, a hydrogen peroxide complex with urea, sodium percarbonate, or mixtures thereof. The whitening agent preferably comprises from about 0.1% to about 50%, even more preferably from about 0.1% to about 5%, and most preferably from about 0.1% to about 2% of the total weight of the oral care composition, depending on the concentration equivalent to the hydrogen peroxide concentration of the selected bleaching agent. In the film, the whitening agent preferably comprises from about 0.01% to about 50%, most preferably from about 0.1% to about 5% of the weight of the film.

[0028] In various embodiments, the active ingredient is an active ingredient in the mouth, which is a non-ionic compound. For example, nonionic antibacterial agents include phenolic and / or bisphenolic compounds, such as halogenated diphenylethers, including triclosan (2,4,4'-trichloro-2'-hydroxy-diphenylether), triclocarbone ((3,4,4-trichlorocarbanilide) , 2-phenoxyethanol, benzoate esters, carbanilides, phenols, thymol, eugenol, hexylresorcinol and 2,2'-methylene bis (4-chloro-6-bromophenol). These antibacterial agents may be present in various amounts, such as from about 0.001 to about 5% by weight of the total weight of the oral care composition.

[0029] The oral care agent may also optionally contain a cationic oral care active ingredient. Cationic active ingredients suitable for use in oral care compositions include, for example:

(i) quaternary ammonium compounds, such as those in which one or two substituents on the quaternary nitrogen have from 8 to 20, preferably from 10 to 18 carbon atoms, and preferably contain an alkyl group, which may optionally be interrupted with an amide, ester, oxygen, sulfur or heterocyclic ring, while the other substituents have fewer carbon atoms, for example from 1 to 7, and are preferably an alkyl group, for example, methyl or ethyl or benzyl. Examples of such compounds include benzalkonium chloride, dodecyl trimethylammonium chloride, benzyl dimethyl stearyl ammonium chloride, hexadecyl trimethylammonium bromide, benzethonium chloride (diisobutyl phenoxyethoxyethyl dimethyl benzyl ammonium chloride) and methyl benzene chloride;

(ii) pyridinium and isoquinoline compounds, including hexadecylpyridinium chloride, alkylisoquinoline bromides; tetradecylpyridinium chloride and N-tetradecyl-4-ethylpyridinium chloride;

(iii) pyrimidine derivatives such as hexetidine (5-amino-1,3-bis- (2-ethylhexyl) -5-methyl-hexahydropyrimidine);

(iv) amidine derivatives such as (4,4'-diamidino-α, (') diphenoxyhexane hexamidine isethionate);

(v) bispridine derivatives, such as octenidine dihydrochloride (N, N '[1,10-decanedildi-1 (4H) -pyridinyl-4-ylidene] -bis- (1-octanamine) dihydrochloride;

(vi) guanides, for example mono-biguanides such as p-chlorobenzyl-biguanide and N '- (4-chlorobenzyl) -N' '- (2,4-dichlorobenzyl) -biguanide, poly (biguanides) such as hydrochloride polyhexamethylene biguanide and bis biguanides of general formula (1):

Α / Χ ^ -Ν-ΟΝΗ-ΟΝΗ- Ητ ^ ^ -ΝΗ-ΟΝΗ-ΟΝ-ίΧ '^ - Α¹

R NH. NH HN HNR¹₍₁) (vii) in which each of the substituents A and A¹ is (i) a phenyl group optionally substituted with (C 1-4) -alkyl, (C 1-4) -alkoxy, nitro or halogen, (ii) a (C 1-12) -alkyl group or (iii ) (C-4-12) -cyclic group; each of X and X substituents¹ is (C-1-3) -alkylene; each of R and R substituents¹ is hydrogen, (C 1-12) alkyl or aryl (C 1-6) alkyl; each of the substituents Z and Z¹ is 0 or 1; n is an integer from 2 to 12; and the polymethylene (CH2) n chain may optionally be interrupted by oxygen or sulfur or by an aromatic radical (e.g. phenyl or naphthyl); and their orally acceptable acid addition salts; examples of such bis-biguanides include chlorhexidine and alexidine. Examples of the acid addition salts of these bis biguanides of general formula (1) include diacetates, dihydrochlorides and digluconates. Suitable chlorhexidine acid addition salts include digluconate, diformate, diacetate, dipropionate, dihydrochloride, dihydrochloride, dimolate, dinitrate, sulfate and tartrate. Suitable alexidine acid addition salts include dihydrochloride and dihydrochloride; and [0030] Other optional oral care agents that are cationic compounds include N alkyl esters^and-acylamino acids and their salts generally represented by the following formula (2):

<img file="PL2046264T3_D0001.tif" />

in which R¹ is an alkyl chain containing from 1 to 8 carbon atoms, preferably ₂ from 1 to 3 carbon atoms and most preferably 3 carbon atoms; R is an alkyl chain containing from 6 to 30 carbon atoms, preferably from 10 to 12 carbon atoms and their₂ mixture; and X is an anion. In various embodiments, the RCO residue includes a natural fatty acid residue, such as a natural fatty acid selected from the group consisting of coconut oil fatty acid, a tallow fatty acid residue, or a single acid fatty acid residue, such as selected from the group consisting of a lauroyl (C12), myristyl residue (C14) and stearoyl (C18) fatty acid and their₂ mixture. In various embodiments, the RCO residue is a lauroyl fatty acid residue.

[0031] X may be any counter-anion that provides a reasonable degree of water solubility (preferably at least about 1 g in 1 liter of water). Examples X include counter-anions that form ester salts of the above formula, inorganic acid salts such as halogen-containing salts (e.g. chloride or bromide) or dihydrogen phosphate or organic salts such as acetate, tartrate, citrate or pyrrolidone carboxylate (PCA). Chloride is preferred.

[0032] Examples of esters of compounds of the above formula wherein n in this formula has a value of 3 that are useful in the oral care compositions of the invention include N-methyl ester salts^and-cocooyl-L-arginine, ethyl ester N^andcocoyl-L-arginine, propyl ester N^and-Cocyclyl-L-arginine, methyl ester N^andstearoyl-L-arginine, ethyl ester N^and-stearoyl-L-arginine, such as the hydrochloride salt. In one embodiment, the cationic oral care agent is lauroyl arginine ethyl ester hydrochloride (ELAH).

[0033] In some embodiments, preferred cationic active ingredients are selected from the group consisting of benzetonium chloride, octenidine, hexetidine, hexamidine, cetylpyridinium chloride, chlorhexidine, alexidine, salts of N alkyl esters^andacylamino acids and mixtures thereof. In some embodiments, the cationic oral care agent is cetylpyridinium chloride (CPC). In some embodiments, the active ingredient for oral care is the N alkyl ester salt^andacylamino acid, such as lauroyl arginine ethyl ester hydrochloride (ALAH). [0034] In some embodiments, the active oral care agent is an anti-stick agent. Without limiting the present invention, it is generally accepted that oral care active ingredients that are non-stick agents either react with the oral surface in such a way that bacteria or biofilm components cannot stick to or react with it. with the bacteria themselves, preventing them from sticking to the surface in the mouth, probably by interacting with adhesins, ligands or other residues on the surface of these bacteria that should normally facilitate binding to the receptor or other surface residue in the mouth. Without limiting the present invention, it is believed that in some embodiments, the N-alkyl ester salts described above^andacyl-amino acids such as lauroylarginine ethyl ester hydrochloride (ALAH) act as an active non-stick component.

[0035] In some embodiments, the active oral care agent is a biofilm destroying agent. A "biofilm destructive agent" is generally a compound that prevents the formation and / or attacks an already formed biofilm (or film) on the surface in the oral cavity and includes enzymes that have the property of hydrolysing proteins, starches and lipids forming part of the biofilm matrix. In some embodiments, such active ingredients are enzymes, including, e.g. proteases such as cysteine ​​proteases or serine proteases. The most preferred enzymes include: papain (e.g. isolated from the juice of green fruits and leaves of Carica papaya), ficin (e.g. isolated from the juice of tropical fig trees Ficus glabrata), krilase (e.g. Antarctic Krill), other cysteine ​​and serine proteases, glucoamylase, dextranase, mutanase, lysozyme, plant lipase, gastric lipase, pancreatic lipase, tannase, bromelain, chymotrypsin, alkalase, amylase, lactoferrin, gsipase and glucidase cellulases, pectinases and mixtures thereof. Other agents that destroy the biofilm in the oral cavity include: synthetic histatin, furanone, furanone derivatives and any mixtures of the above agents.

[0036] In addition to the abovementioned, the oral care compositions of the invention may optionally contain other plaque / plaque destroying agents, including without limitation: sources of copper, magnesium and strontium ions, typically provided in the form of salts; dimethicone copolyols such as cetyl dimethicone copolyol; urea; calcium lactate; calcium glycerophosphate; strontium polyacrylates; and mixtures thereof.

[0037] In some embodiments, the oral care agent comprises an oral care active compound that is an anti-inflammatory agent. Useful anti-inflammatory compounds include flavonoids, flavones, parthenolides such as sesquiterpene lactone-parthenolides, androstenediol (AED) and dehydroepiandrosterone (DHEA). Other useful anti-inflammatory agents include nonsteroidal anti-inflammatory drugs (NSAIDs) such as indomethacin, flurbiprofen, ketoprofen, ibuprofen, naproxen, meclofenamic acid and mixtures thereof. Other suitable anti-inflammatory agents useful as oral care actives include oregano extract (e.g., Origanum vulgare extracts, commonly known as "oregano", "wild oregano" or "marjoram or wild marjoram") as described in U.S. Patent Patent Serial No. 11 / 256.788 to Worrell et al., filed October 24, 2005, or magnolia extract, derived from plants of the Magnoliaceae family, such as Magnolia Officinalis, as reported in US Patent Application Serial No. US 11 / 285,809 to Gaffar et al. filed November 23, 2005.

[0038] A preferred oral care active ingredient comprises a combination of at least one flavonoid and at least one flavone such as in the product UNIVESTIN®, manufactured and sold by Unigen Pharmaceuticals, Inc. (Superior, CO. United States of America). A full description of the UNIVESTIN® product is found in U.S. Patent Application Publication 2003/0216481, owned by Jia.

[0039] Examples of antioxidants useful as active ingredients in the mouth include butylhydroxyanisole (BHA), butylhydroxytoluene (BHT), vitamin A, carotenoids, tocopherols (vitamin E), flavonoids, polyphenols, ascorbic acid (vitamin C), herbal antioxidants melatonin, chloride, calcium, calcium oxide, calcium chloride, ubiquinone disodium (coenzyme Q10), ethylhexyl gallate, hydrogen peroxide, iodine, lycopene, magnesium ascorbate, potassium sulfite, sodium bisulfite, thiomylic acid and mixtures thereof. In some embodiments, the oral care compositions comprise an antibiotic active ingredient in the oral cavity such as augmentin, amoxicillin, tetracycline, doxycycline, minocycline, metronidazole, neomycin, kanamycin and clindamycin, and mixtures thereof.

[0040] Other useful oral active ingredients include sources of fluoride ion, preferably present in an amount sufficient to provide from about 25 ppm to about 5000 ppm fluoride ions, such as sodium fluoride, potassium fluoride, sodium fluorosilicate, ammonium fluorosilicate, monofluorophosphate sodium (MFP) and amine fluorides, including olaflur (N'-octadecyltrimethylenediamine-N, N, N'15 tris (2-ethanol) dihydrochloride). Suitable stannous (tin (II)) sources include, without limitation: stannous fluoride, stannous other halides such as stannous chloride dihydrate, stannous pyrophosphate, tin (II) organic carboxylate salts such as formate, acetate, gluconate, lactate, tartrate, stannous malonate and citrate, tin (II) ethylene glycol and the like. One or more stannous ion sources are optionally and, for example, present in a total amount from about 0.01% to about 10%. Sources of zinc ion, such as zinc acetate, zinc chloride, zinc citrate, zinc gluconate, zinc glycinate, zinc oxide, zinc sulfate, sodium zinc citrate and the like are present, for example, in a total amount of from about 0.05% to about 3%.

[0041] Some types of useful anticalculus active ingredients have the structure of linear molecularly dehydrated polyphosphate salts. Polyphosphate salts are generally used in the form of water-soluble salts, completely or partially neutralized with an alkali metal (i.e. in the form of potassium, sodium or ammonium salts and mixtures thereof). Thus, linear, dehydrated polyphosphate compounds useful as anticalculus agents include, for example, sodium tripolyphosphate, sodium hexametaphosphate, pyrophosphate, alkali metal di- or tetra-pyrophosphate salts such as Na4P2O7, K4P2O7, Na2K2P2H2P2O2, cyclic, such as sodium tripolyphosphate, sodium trimetaphosphate or mixtures thereof. In various embodiments, these anticalculus active ingredients are present in the bulk of the oral care composition of the invention at concentrations from about 0.001 to about 10%, more preferably from about 1 to about 5%.

[0042] As agents that increase the effectiveness of certain oral care active ingredients, including antimicrobial, anticalculus or other active ingredients in the oral care composition, synthetic anionic linear polycarboxylates are also known. In addition, these compounds can also be used to make films as described below. Such anionic polycarboxylates are generally used in the form of free acids or preferably in the form of partially neutralized and more preferably completely neutralized water-soluble alkali metal (e.g. potassium and preferably sodium) salts or ammonium salts. Preferred copolymers are copolymers from 1: 4 to 4: 1 anhydride or maleic acid with another polymerizable ethylenically unsaturated monomer, preferably methyl vinyl ether (methoxyethylene) with a molecular weight (MW) from about 30,000 to about 5,000,000. The preferred copolymer is copolymer (methyl vinyl ether / maleic anhydride). Examples of useful copolymers are marketed by ISP Corporation under the trade name GANTREZ®, e.g. AN 139 (MW 1,100,000), AN 119 (MW) 200,000); S-97 of pharmaceutical grade (1,500,000 MW), AN 169 (2,000,000 MW) and AN 179 (2,400,000 MW); the preferred copolymer is S-97 for pharmaceutical purposes (MW 1,500,000). In various embodiments, if a synthetic anionic polycarboxylate is included in the oral care composition, it is preferably present in an amount of from about 0.001% to about 5% by weight.

[0043] Salivary secretagogues (including food acids such as citric, lactic, maleic, succinic, ascorbic, adipic, fumaric and tartaric acids, and mixtures thereof) may also be present. Other useful active ingredients are histamine H2 receptor antagonists. H2 antagonists useful in the invention include cimetidine, etinididine, ranitidine, ICIA-5165, thiotidine, ORF17578, lupitidine, donetidine, famotidine, roxatidine, pifatidine, lamididine, BL6548, BMY-25271, zalididine, m-idis -94482, BL6341A, ICI-162846, ramixotidine, Wy-45727, SR-58042, BMY-25405, locstidine, DA4634, bispentidine, sulfotidine, ebrotidine, HE-30-256, D-16637, FRG-8813, FRG8701, impromidine , L-643728, HB-408.4 and mixtures thereof. De-sensitizing agents useful in the invention include potassium citrate, potassium chloride, potassium tartrate, potassium bicarbonate, potassium oxalate, potassium nitrate, strontium salts and mixtures thereof. Alternatively or additionally, one or more topical or general analgesics can be used, such as aspirin, codeine, acetaminophen, sodium salicylate, or triethanolamine salicylate.

[0044] Suitable nutrients include vitamins, minerals, amino acids and mixtures thereof. Preferred vitamins are vitamins C and D, thiamin, riboflavin, calcium pantothenate, niacin, folic acid, nicotinamide, pyridoxine, cyanocobalamin, para-aminobenzoic acid, bioflavonoids and mixtures thereof. Nutritional supplements include amino acids (such as L-tryptophan, L-lysine, methionine, threonine, levocarnitine and L-carnitine), lipotropic agents (such as choline, inositol, betaine and linolenic acid), fish oil (including its components like polyunsaturated fatty acids omega-3 (N3), eicosapentaenoic acid and docosahexaenoic acid) and mixtures thereof.

[0045] Non-limiting examples of personal care active ingredients include surface active agents, skin conditioners, hair and nails conditioners (e.g. silicone oils, cationic silicones, silicone resins, silicones and silicone resins with a high refractive index and organic conditioning oils (such as hydrocarbon oils, polyolefins and fatty acid esters), skin and scalp sensitizers, astringents, soothing agents and hairy scalp, skin healing agents, moisturizers, emollients, skin whitening agents, antibacterial agents, anti-inflammatory agents, unpleasant odors, anti-aging agents, anti-acne agents, anti-psoriasis agents, anti-dandruff agents, skin fat liquefying agents, wetting agents, active agents as deodorants, active agents as antiperspirants, natural extracts and essential oils, nutrients, occlusive agents, enzymes, proteins, amino acids, vitamins, painkillers, sunscreens and UV absorbers (e.g. 2-ethylhexyl p-methoxycinnamate, 2-ethylhexyl N, N-dimethyl-paminobenzoate, p-aminobenzoic acid, 2-phenylbenzimidazole-5-sulfonic acid, octocrylene, oxybenzone, homomentyl salicylate, octylmethyl-salylate, 4,4'-methyloxy , 4-isopropyl-dibenzoylmethane, 3-benzylidene camphor, 3- (4-methylbenzylidene) camphor, titanium dioxide, zinc oxide, silica, iron oxide), antioxidants, antibiotics, exfoliating agents, chelating agents, dyes (including suitable dyes such as non-oxidative dyes, including 'direct dyes', metal dyes, metal chelate dyes, dyes acting on fibers and other synthetic and natural dyes), opacifiers, tanning agents, biocides, analgesics ( Outside). Many of these active ingredients are the same as described above in the context of oral care. Other ingredients known to those skilled in the art are also contemplated.

[0046] Cationic surfactants such as quaternary ammonium salts are used in hair rinses and shampoos as conditioning agents, as well as various silicones and other water-insoluble conditioning agents, including waxes, greases and oils. Non-limiting examples of fiber conditioning agents include organosilicon compounds, e.g. non-volatile silicones (especially aminosilicones); Polyethylene; paraffin; Vaseline; microcrystalline waxes; fatty acids and triglycerides, for example C18-36- (mixed) fatty acids, stearyl stearate; and quaternary ammonium salts and amine salts (which also act as surfactants). Exemplary personal care compositions and active ingredients are described in US Patent Nos. US 5,213,716 (Patel et al.), US 6,955,817 (McAtee et al.), US 6,835,373 (Kolodzik et al.) And US 6,974,799 (Lintner).

[0047] Liquid cleansing compositions include active ingredients such as cleansing surfactants, including anionic, cationic, nonionic and amphoteric surface-active soaps, detergents (such as sulfates, e.g. sodium sulfate), phosphates (e.g. trisodium phosphate, disodium phosphate), complex phosphates (e.g. tetrasodium pyrophosphate, sodium tripolyphosphate, sodium tetrafosphate, sodium hexametaphosphate), silicates (e.g. sodium silicate, colloidal silicates), carbonates (e.g. sodium carbonate, sodium bicarbonate), polymeric detergents, bleaching compounds (e.g. sodium hypochlorite, sodium perborate, sodium percarbonate), activators, pH buffering agents, enzymes, conditioning agents, diluents, chelating agents, enzymes, polymers preventing secondary deposition, polymers releasing dirt, polymeric dispersants and / or dirt suspenders, movement inhibitors dye, fabric integrity protectors, anti-foam agents, fabric softeners, flocculants, fragrances, bleaching agents and combinations thereof. Active ingredients useful in household compositions include, for example, detergent surface-active ingredients, detergents, conditioners, natural extracts and essential oils, enzymes, proteins, amino acids, dirt release agents, bleaching agents, antibacterial agents, liquidation agents unpleasant smells and fabric softeners. Exemplary cleaning and household products are described in US Patents US 6,670,318 (Hokkirigawa et al.), US 5,294,364 Thomas et al., US 4,869,842 (Denis et al.), US 3,965,026 (Lancz), in US 2003/0082131 (Drapier) and US 2005/0272628 (Meli) and in PCT / WO 97/11151.

[0048] Useful films of the invention may be rigid or flexible and may contain any variety of materials, including film-forming materials, clays, waxes and mixtures thereof. In some embodiments, the film contains at least one film-forming material, preferably a polymer. Useful polymers include hydrophilic and hydrophobic polymers. In some embodiments, the polymer is soluble in a solvent such as water. A water-soluble polymer that dissolves upon contact with water and physical force during use is desirable (such as when brushing teeth or scrubbing with a brush or spatula). In some embodiments, the polymer is insoluble but crumbles in water and disperses, i.e. the polymer breaks down into small fragments by mechanical or shear force. In some embodiments, the polymer is insoluble but swells. If the polymer does not disintegrate completely during use, it may be a water-wet polymer or a water-stable hydrophilic polymer, such as some types of cellulose, e.g. paper. Examples of useful polymers are described in US Patent Nos. US 4,713,243 (Schiraldi et al.), US 6,419,903, US 6,419,906, US 6,514,483 (all belonging to Xu) and US 6,699,929 (Boyd et al.); in US Patent Publication Nos. 2004/0126332, US 2004/0136924 and US 2004/0042976 (all belonging to Boyd et al.) and US 2004/0062724 (Moro et al.).

[0049] Preferably, the polymers are selected and separated in the film to provide at least one of the following characteristics: (1) the desired stability of the film containing the active ingredient in the carrier, (2) the desired degree of film disintegration when applying the composition, or (3) the desired degree exposure of the active ingredient when applying the composition.

[0050] In preferred embodiments, the film is water-soluble, including, for example, a water-soluble polymer, a water-dispersible polymer, or a water-insoluble polymer with an optional water-soluble filler. The relative amounts of water-insoluble polymer, water-soluble polymer or optionally water-soluble filler can be selected so that the amount of active ingredient released is proportional to how vigorously or how long the composition will be used, e.g. by brushing, scrubbing or other mechanical activity during applying this aqueous composition.

[0051] It is noted that various embodiments of the invention relate to films provided in the form of multiple fragments, tapes, sheets and the like; a film containing the active ingredient may also be suitable as a material for encapsulating various components. The encapsulation film may also be able to transfer the active ingredient from the medium in accordance with the principles set out in the present invention.

[0052] In some embodiments, the polymer is a water-soluble polymer. An example is a cellulose ether polymer such as hydroxyalkyl alkyl cellulose, including hydroxypropyl methyl cellulose (HPMC) commercially available from the Dow Chemical Company of Midland, MI, United States of America as products called

METHOCEL®, including, for example, METHOCEL®E5, METHOCEL®E5LV, METHOCEL®E50, METHOCEL® E15 and METHOCEL® K100, hydroxypropyl cellulose (HPC), hydroxyethyl cellulose (HEC), methyl cellulose (MC), carboxymethyl cellulose and mixtures thereof. Other useful polymers include polyvinylpyrrolidone (PVP), which may have a weight average molecular weight of about 100,000 or more, up to about 1.5 million, vinyl acetate copolymers, polyvinylpyrrolidone-vinyl acetate, such as KOLLIDON® VA64 supplied by BASF, in a proportion 60:40 vinyl / pyrrolidone) and PLASDONE® S630 PVP (supplied by International Specialty Products, Wayne, NJ, United States of America, 60:40 vinylpyrrolidone: vinyl acetate), ethylene oxide grafted PVA copolymers such as

KOLLICOAT® IR (supplied by BASF, 75% by weight PVA, 25% by weight polyethylene glycol grafted poly (vinyl alcohol) (PVA), acrylates and polyacrylic acid, including polyacrylate polymer, cross-linked polyacrylate polymer, cross-linked poly (acrylic acid) ( e.g. CARBOPOL®, vinylcaprolactam / sodium acrylate polymers, methacrylates, poly (vinyl alkyl ether 20 maleic acid) maleic copolymer (e.g. GANTREZ®), copolymers of vinyl acetate and crotonic acid, polyacrylamide, poly (2-acrylamido-2-methylpropanesulfonate), terpolymers of monomers: acrylic methyl propylsulfonic acid / methyl acrylate / styrene, phosphonostyrene polymers, polyethylene phosphonate, polyphosphonate, polybutophosphonate polyalkylenes, poly (alkylene oxides) including poly (ethylene oxide), i.e. polyethylene glycol and carboxyvinyl polymer. It is obvious to those skilled in the art that the film may also contain derivatives, copolymers and further mixtures of these polymers.

[0053] Useful water insoluble polymers include polymers soluble in at least one organic solvent; for example acrylic copolymers (in which the carboxylic acid function is not neutralized), cross-linked polyvinylpyrrolidone, for example KOLLIDON® CL or CL-M, supplied by BASF, polyvinyl acetate (PVAc), some cellulose derivatives such as cellulose acetate , cellulose nitrate, alkyl cellulose such as ethyl cellulose, butyl cellulose and isopropyl cellulose, cellulose acetate phthalate, shellac, ethylene-vinyl acetate copolymers, vinyl acetate homopolymer, silicone polymer (e.g. dimethylsilicon), poly (methyl methacrylate) (PMMA), polymers insoluble in organic solvents such as cellulose, polyethylene, polypropylene, polyesters, polyurethane and nylon, natural and synthetic rubber, and mixtures thereof. An example of a suitable film-forming acrylic copolymer is

LUVIMER® 30E, 30% (by weight) solution of copolymer (tert-butyl acrylate / ethyl acrylate / methacrylic acid) in ethanol supplied by BASF (Florham Park, NJ, USA). These water insoluble polymers can be prepared in the form of dispersions (e.g. by emulsion polymerization) and can be stabilized with suitable emulsifiers. A useful PVAc emulsion is, for example, KOLLICOAT®

SR 30D, 30% (by weight) PVAc dispersion in water stabilized with 2.7% by weight PVP and 0.3% sodium lauryl sulfate. An example of an acrylic copolymer dispersion is KOLLICOAT® EMM 30D, 30% (w / w) aqueous copolymer dispersion: ethyl acrylate: methyl methacrylate (with a weight ratio of ethyl acrylate to methyl methacrylate of about 2: 1) with a declared average molecular weight of about 800,000, supplied by BASF .

[0054] Other useful water-soluble polymers or fillers include, without limitation, natural resins such as sodium alginate, carrageenan, xanthan gum, acacia, acacia, guar gum, pullulan, agar, chitin, chirozan, pectin, karaja gum, zein, hordein, gliadin, carob gum, tragacanth and other polysaccharides; starches such as maltodextrin, amylose, high amylose starch, corn starch, potato starch, rice starch, tapioca starch, pea starch, sweet potato starch, barley starch, wheat starch, waxy starch, e.g. modified starch, e.g. high amylose starch), dextrin, levan, elsinan and gluten; and proteins such as collagen, isolated wheat protein, casein, milk protein, soy protein, keratin and gelatin. The film may also contain dispersed or swelling fillers, such as modified starch, alginate esters, alginate salts with divalent or polyvalent ions.

[0055] Further non-limiting examples of water-insoluble polymers include cellulose acetate, cellulose nitrate, ethylene-vinyl acetate copolymers, vinyl acetate homopolymer, ethyl cellulose, butyl cellulose, isopropyl cellulose, shellac, hydrophobic silicone polymer (e.g. dimethylsilicon), PMMA (poly (methyl methacrylate)), cellulose acetate phthalate and natural or synthetic resins; polymers insoluble in organic solvents such as cellulose, polyethylene, polypropylene, polyesters, polyurethane and nylon.

[0056] In the aqueous composition, the relative amounts of the water-soluble polymer to the water-insoluble polymer and / or the partially water-soluble polymer in the film are preferably chosen such that the film is stable during storage in the aqueous composition but breaks down when using this composition. In various embodiments, the film comprises a water-soluble polymer in an amount ranging from about 0.1% to about 90%, from about 1% to about 80%, from about 5% to about 70%, from about 9% to about 50% or from about 10% to about 40% by weight based on the weight of the film. In addition to or instead of the water-soluble polymer (s), the film may contain partially water-insoluble or water swellable polymers in an amount of from about 0.1% to about 50% by weight of the film, preferably from about 1% to about 10% by weight. In various embodiments, the method of stabilizing hydrophilic films in the aqueous medium of the carrier uses water-soluble and insoluble materials in the film, so balanced that the film maintains stability during storage in the product carrier but disintegrates during use, releasing the component contained therein active.

[0057] Preferably, the film of the invention optionally contains optionally one or more of the following additional ingredients: surfactants, viscosity modifiers, thickeners, humectants, diluents, fillers (in addition to those described above), pH modifying agents, plasticizers, fillers , waxes, texture modifiers, oils, flavors and / or sweeteners, preservatives, solvents and mixtures thereof. It is understood that although the general characteristics of each of the above categories of materials may be different, there may be some common characteristics and each specific material may serve many purposes within two or more categories of materials.

[0058] One or more surfactants in the film may perform the function of a surfactant, emulsifier and / or foam modulator. Surfactants or surfactants are conventionally used in a wide variety of oral care formulations, providing solubilization, dispersion, emulsification and wetting of other components present, especially essential oils. In various implementations, surfactants contribute to the increase of prophylactic effect by thoroughly dispersing the active ingredients in the film mass and in some cases in the surrounding environment when the film dissolves. In addition, in various embodiments, surfactants can improve the cosmetic appearance of the film composition. Suitable surfactants and emulsifying agents are preferably those that are rationally stable over a wide pH range, including non-soap organic synthetic anionic, nonionic, bipolar and amphoteric detergents. In some embodiments, the one or more surfactants are present in the film composition in an amount ranging from about 0.001% to about 5%, more preferably from about 0.5% to about

5% and most preferably from about 1% to about 3% by weight of the film.

[0059] Nonionic surfactants useful in the compositions of the invention include compounds produced by condensation of alkylene oxides (especially ethylene oxide) with an organic hydrophobic compound which may have an aliphatic or alkylaromatic structure. One group of surfactants is known as "ethoxamers" - condensation products of ethylene oxide with fatty acids, fatty alcohols, fatty acid amides, polyhydric alcohols (e.g. sorbitan monostearate) and the like. The term "polysorbates" describes a class of nonionic surfactants produced by ethoxylation of free hydroxyl groups in fatty acid sorbitan esters. They are marketed, for example as TWEEN® surfactants by ICI America, Inc. (Bridgewater, New Jersey, USA) .. Non-limiting examples include Polysorbate 20 (sorbitan polyoxyethylene monolaurate 20, TWEEN® 20) and Polysorbate 80 (sorbitan polyoxyethylene monooleate 20, TWEEN® 80). Preferred polysorbates are those having from about 20 to about 60 moles of ethylene oxide per mole of sorbitan ester.

[0060] Other suitable nonionic surfactants include block copolymers of poly (oxyethylene) poly (oxypropylene), especially triblock polymers of this type with two blocks of poly (oxyethylene) and one block of poly (oxyethylene). Such copolymers are known commercially under the common name poloxamers, the name being given together with the numerical suffix identifying each individual copolymer. Poloxamers can have different contents of ethylene oxide and propylene oxide, which gives a wide range of chemical structures and molecular weights. A preferred poloxamer is Poloxamer 407, which is widely available, for example under the trade name Pluronic® F127 (BASF Corporation, Florham Park, NJ, United States).

[0061] Other non-limiting examples of suitable nonionic surfactants include products derived from the condensation of ethylene oxide with the reaction product of propylene oxide and ethylenediamine, long chain tertiary amine oxides, long chain tertiary phosphine oxides, long chain dialkyl sulfoxides and similar compounds.

[0062] In the embodiments of the invention, synthetic bipolar surfactants may also be useful. Some of them can be broadly described as derivatives of aliphatic quaternary ammonium, phosphonium and sulfonium compounds, in which the aliphatic radicals may have a straight or branched chain and in which one of the aliphatic substituents contains from 8 to 18 carbon atoms and one contains an anionic group that gives water solubility for example. carboxyl, sulfonate, phosphate or phosphonate group. An example of a suitable bipolar surfactant is 4- (N, N-di (2-hydroxyethyl) -N-octadecylammonium) -butane 1-carboxylate.

[0063] Other suitable zwitterionic surfactants include betaine surfactants such as those described in US Patent 5,107,577 (Polefka et al.). Typical alkyldimethyl betaines include decylbetaine (2- (N-decyl-N, N-dimethylammonium acetate)), cocobetaine, myristylbetaine, palmitylbetaine, laurylbetaine, cetylbetaine, stearylbetaine and similar compounds. Examples of amidobetaines are cocoamidoethyl betaine, cocamidopropyl betaine, lauramidopropyl betaine and the like. Cocamidopropyl betaine and lauramidopropyl betaine are particularly useful betaine surfactants.

[0064] Examples of suitable anionic surfactants are the water soluble salts of monoglyceride monosulfonates of higher fatty acids, such as the sodium salt of monosulfonated monoglyceride of hydrogenated coconut oil fatty acids, higher alkyl sulfates such as sodium lauryl sulfate (SLS), alkylaryl sulfonates such as sodium dodecylbenzene sulfonate, higher alkyl sulfoacetates, higher fatty acid esters with 1,2-dihydroxypropane sulfonate and substantially saturated higher aliphatic acylamides of lower aliphatic aminocarboxylic acids, such as those having 12 to 16 carbons in fatty acid, alkyl or acyl radicals and the like. Examples of recently mentioned amides are N-lauroyl sarcosine and the sodium, potassium and ethanolamine salts of N-lauroyl, N-myristoyl or N-palmitoyl sarcosine, which are preferably substantially free of soap or similar higher fatty acid material. [0065] The film optionally contains one or more plasticizers that allow the strength and flexibility of the film to be adjusted. Typically, the plasticizer reduces film stiffness. Plasticizing compounds may include glycols such as propylene glycol or a low molecular weight polymer, for example polyethylene glycol such as any of the CARBOWAXES ™ group with a molecular weight from about 200 to about 600, supplied by Dow Chemical. Polyhydric alcohols such as glycerin or propylene glycol, sorbitol, xylitol, glycerol esters such as glycerol triacetate (triacetin), triethyl citrate and natural oils such as mineral oil, castor oil and vegetable oils can also be used. Such plasticizers optionally comprise from about 1% to about 50%, from about 5% to about 30%, or from about 10% to about 25% by weight of the film.

[0066] Bulk agents, bulking ingredients or viscosity modifiers may modify the properties of films and may also be present therein. Such thickeners may include water-insoluble inorganic materials that may be in the form of particles, such as, for example, silicon dioxide (silica), tricalcium phosphate, dicalcium phosphate (calcium monohydrogen phosphate), calcium carbonate, nacre and clays. Water-insoluble organic thickeners may include cellulose, polyethylene, polypropylene and various starches from potato, corn, oats, rice, wheat or tapioca and modified food starches such as, for example, maltodextrin. The thickeners may optionally be present in an amount of from about 1% to about 50%, from about 5% to about 30%, or from about 10% to about 25% by weight based on the weight of the film.

[0067] Non-limiting examples of suitable additional components include clays, compounds containing a hydrophobic organic non-polymeric material such as wax (e.g. beeswax or paraffin), texture modifiers such as cold water swellable, physically modified and pregelatinized starches and dyes . In some implementations, the film contains graphite.

[0068] In various embodiments, the film contains a formulation dye to give color to this film, composition or both. In some embodiments, film fragments contrast with the carrier and are white, black or any color that is visible on the background or contrasts with the background of the carrier. Useful formulation dyes include non-toxic, water-soluble dyes, or pigments, such as, for example, metal oxide "lakes". In some embodiments, the dye is legally authorized for incorporation in a food or drug by a government agency, such as FD&amp;C pigments or dyes or D&amp;C approved by the FDA for use in the United States. Useful dyes include FD&amp;C Red No. 3 (tetrajodofluorescein sodium), Food Red 17, 6-hydroxy-5 - {(2-methoxy-5-methyl-4-sulfophenyl) azo} -2-naphthalenesulfonic acid sodium salt, Food Yellow 13, sodium salt of a mixture of quinophthalon mono- and disulfonic acids or 2- (2-quinolyl) indanedione, FD&amp;C Yellow No. 5 (4p-sulfophenylazo-1-p-sulfophenyl-5-hydroxypyrazole-3-carboxylic acid sodium salt), FD&amp;C Yellow

Well. 6 (sodium p-sulfophenylazo-e-naphthol-6-monosulfonate), FD&amp;C Green No. 3 (4 - {[4- (N-ethyl-p-sulfobenzylamino) -phenyl] - (4-hydroxy-2-sulfonium-phenyl) methylene} - [- 1- (N-ethyl-Np-sulfobenzyl) disodium salt -A-3,5-cyclohexadieneimine], FD&amp;C Blue No. 1 (disodium salt of dibenzyldiethyl diaminotriphenylcarbino-1-trisulfonic acid anhydride), FD&amp;C Blue No. 2 (indigo carmine disulfonic acid sodium) and mixtures thereof in various proportions. In one embodiment, the dye is a water insoluble inorganic pigment, such as titanium dioxide, green chromium oxide, phthalocyanine green, ultramarine blue, iron oxide or water insoluble dye lakes. In some embodiments, the dye lakes include FD&amp;C dye calcium or aluminum salts, such as FD&amp;C Green # 1 lacquer, FD&amp;C Blue # 2 lacquer, D&amp;C Red # 30 lacquer or FD &amp; C # Yellow 15 lacquer. In some embodiments, the water-soluble dye such such as FD&amp;C Blue # 1, is contained in a water-insoluble polymer, such as, for example, polyethylene, such as found in polyethylene beads (e.g., Microblue Spectrabeads, marketed by Micropowders, Inc.). In some implementations, the film contains a dye such as D&amp;C Red # 30. In some embodiments, a white dye is used, e.g., titanium dioxide (TiO2), titanium dioxide-coated mica (e.g., Timiron), mica, mineral, or clay. In some embodiments, the dye is a non-permeable dye (non-staining). In various embodiments, the film contains a dye at a level of from about 0.5% to about 20% by weight of the film or from about 1% to about 15% by weight of the film or from about 3% to about 12% by weight based on the weight of the film.

[0069] In some embodiments of the invention, the film for use in oral care compositions contains one or more flavoring agents, which may include any agents known to those skilled in the art, such as natural and artificial flavors. These fragrances can be synthetic fragrance oils and fragrances, and / or oils, oleoresins and extracts derived from plants, leaves, flowers, fruits etc. and mixtures thereof. In some embodiments, the fragrance is an essential oil, extract or fragrance aldehyde, ketone, ester or alcohol that impart the fragrance; it is selected from the group consisting of peppermint leaf oil, peppermint oil, wintergreen, sassafras, clove, sage, eucalyptus, marjoram, cinnamon, lemon, lime, grapefruit, orange, apple, pear, peach, strawberry, cherry, apricot oil , watermelon, banana, coffee, cocoa, menthol, carvone, anethole and mixtures thereof. Representative fragrance oils include: mint leaf oil, cinnamon oil, peppermint oil, clove oil, faba oil, thyme oil, cedar leaf oil, nutmeg oil, oil and bitter almond oil. Also useful are artificial and natural or synthetic fragrances, such as vanilla, chocolate, cola, coffee, cocoa citrus oil, including lemon, orange, grape, lime, grapefruit and fruit essences, including apple, pear, peach, strawberry , wild strawberry, cherry, plum, pineapple, apricot and the like, singly or in combinations. In various embodiments, the aroma is incorporated into the film in an amount of from about 0.01% to about 10% by weight based on the weight of the film.

[0070] In some embodiments, the composition is an oral care composition in which the sweetener is used alternatively or complementarily to the fragrance. Suitable sweeteners are water-soluble and include sodium saccharin, sodium cyclamate, xylitol, perilartien, D-tryptophan, aspartame, sucralose, dihydrochalkones and the like, at concentrations from 0.01 to about 1% of the film. Most preferably, the sweetening material is sodium saccharin.

[0071] In some embodiments of the invention, the film is porous. In the present invention, "porous" means that it has many pores dispersed in mass. Preferably, in some embodiments, the pores have open cells, and therefore, the pores dispersed in the bulk of the film open to each other, forming continuous paths or channels in the bulk of the film, allowing the entry and exit of solvents and / or active ingredients. These pores can be macroporous (i.e. their average size is greater than about 50 nm), mesoporous (i.e. their average pore size is from about 2 to about 50 nm) or microporous (i.e. their average pore size is less than 2 nm or 20 Angstroms).

[0072] As stated above, preferred embodiments of the invention provide methods for incorporating the active ingredient into a film by transferring at least a portion of the active ingredient in the medium that contains the active ingredient. As described above, initially the film essentially does not contain the active ingredient to be transferred. The film can be made to contain many active ingredients and so that only selected active ingredients pass from the medium to this film. There is a gradient of active ingredient concentration between the medium and the film. Preferably, the medium is a liquid or semi-solid phase, although other phases such as a gas or solid phase are contemplated. At least part of the active ingredient present in the medium is transferred to the film. This can be done by passive mass transport, such as diffusion of the active ingredient using a concentration gradient with transfer of the active ingredient to the film under mild conditions. Alternatively, some form of external energy utilized in this system may be involved in the transfer, for example, to accelerate thermodynamic equilibrium, to increase the transfer rate of the active ingredient, to overcome energy or mass transfer barriers, and the like. Active application of external factors includes, for example, the use of electricity, heat and pressure.

[0073] During the transfer process, the film contacts the medium. The film is immersed in the medium to maximize the exposed surface in order to facilitate the greatest possible contact with the medium, and thus the transfer of the active compound. Optionally, the medium containing the film can be mixed continuously or intermittently. The transfer process can be carried out in a batch or continuous process.

[0074] In preferred embodiments, the medium is a liquid phase or a semi-solid phase (e.g., gel, paste). The medium contains the active ingredient and preferably has at least one phase in which the active ingredient is dispersed. This active ingredient may be suspended and / or solvated in at least one phase in this medium. The active ingredient may be in a discontinuous phase in this medium. As known to those skilled in the art, the medium may consist of multiple phases, and may be an emulsion or other multiphase system. For example, if the active ingredient is lipophilic it may be dispersed in the lipophilic phase. Similarly, the hydrophilic active ingredient is preferably dispersed in a compatible hydrophilic phase. The medium may contain one or more solvents (polar or non-polar) or suspensions (aqueous or non-aqueous).

[0075] In some embodiments, as described in more detail below, the carrier for oral care compositions, personal care compositions, cleaning compositions and / or household compositions is a medium containing the active ingredient following the transfer of at least a portion of the active ingredient . In such embodiments, the medium is selected to contain components compatible with the intended use, which may include choosing the carrier components according to the particular composition. In some embodiments, the medium contains an amount of polar solvent, such as water, from 5% to about 95% by weight. Other non-limiting components include additional solvents, polyhydric alcohols, wetting agents, thickening agents, surfactants and other components known to those skilled in the art. In some embodiments, the medium contains a polyhydric alcohol such as glycerin, which can be combined with other solvents such as water.

[0076] In various embodiments, the active ingredient is transferred at a concentration above about 0.01%, optionally above about 1%, optionally above about 5%, optionally above about 10%, optionally above about 20%, optionally above about 30%, optionally above about 50% and optionally above about 75%.

[0077] Preferably, at least part of the active ingredient is transferred from the medium to the film. It is recognized by those skilled in the art that the duration of the transfer may vary depending on the amount of active ingredient present in the medium, the desired concentration of active ingredient in this film, and the method of production. In some embodiments, the medium is used as a carrier for the final composition or product. Thus, the carrier of this composition is optionally a medium. In addition, in some implementations, the medium creates the medium for this composition. The carrier may further contain one or more additional active ingredients, regardless of those to be transferred to the film. In other embodiments, the medium is a transfer medium used to transfer the active ingredient to the film, but the medium is not then used in the resulting composition / product.

[0078] It is understood by those skilled in the art that the concentration of the medium is dependent on the final use. For example, where the medium will be introduced into the carrier, the concentration of the active ingredient is optimized to be within the desired concentrations that are both effective and non-toxic at which an effective amount of the active ingredient is achieved. In addition, in this case, the medium will be in contact with the carrier during storage of the composition, so the duration of the transfer will be relatively long, which will allow the concentration gradient to reach equilibrium (or allow irreversible uptake of the active ingredient by this film). The degree of dilution of the medium in the carrier will also be dictated by the required concentration of active ingredient in this medium (hereinafter giving the desired concentration of active ingredient in the film). In other implementations, e.g., in which the medium is only a transfer medium, the concentration of the active ingredient can be relatively high to facilitate a larger concentration gradient and faster transfer of the active ingredient to the film.

[0079] In some embodiments, the transfer occurs under ambient conditions. In some embodiments, the transfer occurs at a temperature greater than or equal to about 25^aboutC. Further, in some embodiments, the transfer takes place in less than about 10 hours, optionally less than about 5 hours, optionally less than about 3 hours, optionally less than about 1 hour, and optionally less than 30 minutes. In some embodiments, the transfer takes place in less than about 20 minutes, optionally less than about 15 minutes, and optionally less than about 10 minutes. In other embodiments, the transfer takes about 10 to 72 hours or lasts longer. In one embodiment, the transfer takes place in less than about 48 hours, for example about 24 hours. In one embodiment, the medium contains as active ingredient hydrogen peroxide in an aqueous solution in which the concentration of hydrogen peroxide is from about 1 to about 50% by weight, from about 1 to about 10%, optionally from about 1 to about 5% by weight. Initially, the film does not contain bleaching hydrogen peroxide. After 24 hours, the film contains from about 0.01% to about 10% hydrogen peroxide, optionally from about 1% to about 5% by weight based on the weight of the film.

[0080] Thus, in some embodiments it is preferred that the portion of the transferred active ingredient present in the film after the transfer is greater than about 0.01%. In other embodiments, the amount of transferred active ingredient present in the film is greater than about 1%, optionally greater than about 5%, optionally greater than about 10%, optionally greater than about 20%, optionally greater than about 30%, optionally greater than about 40%, optionally greater than about 50%, optionally greater than about 60%, and optionally greater than about 75%. However, as will be appreciated by those skilled in the art, the concentration of active ingredient in the film may be very low, for example where an aroma, sweetener, dye or highly active agent is used. In addition, the concentration of the active ingredient in the film depends on many different factors, including the effective amount of the active ingredient and the tendency of the film to accept and maintain the active ingredient, which in turn may depend on many different factors, including but not limited to film porosity, chemical compatibility between film and the active ingredient.

[0081] The films of the invention preferably have a substantially lamellar structure. The "lamellar" structure is characterized by a size in one or two dimensions (eg dimensions x- or y) significantly greater than the thickness of the structure in the third dimension (ie in the dimension z-) and generally includes, for example, flat, layered or lamellar shapes . In one embodiment, the lamellar structure is essentially flat and has a size in both x- and y-dimensions significantly greater than in the z-dimension. In other embodiments, the lamellar structure is not flat.

[0082] Expressing this in a different way, the films preferably have an aspect ratio (elongation) of about 5: 1 or greater. Generally, the aspect ratio (AR) is defined as AR = L / D, where L is the length of the longest dimension and D is the length of the shortest dimension. In some implementations, the film fragments have an aspect ratio of at least about 10: 1. In various implementations, film fragments have an aspect ratio of about 5: 1 to about 10,000: 1. In one embodiment, the film is a substantially continuous surface, which may appear to be a substantially flat surface, although in some implementations, the film may be deformed. In such implementations, the film can have any number of shapes, including a smooth, bent surface. In addition, the term "film" includes both a single structure and multiple film fragments. In some embodiments, the film is a plurality of fragments having an independent thickness from about 2.54 μm (0.1 mils) to about 254 μm (10 mils), preferably from about 12.7 μm (0.5 mils) to about 229 μm ( 9 mils) and more preferably from about 30.5 μm (1.2 mils) to about 76.2 μm (3 mils). The preferred length of the fragments is at least about 0.2 mm.

[0083] In various implementations, the film consists of many fragments or parts. Such fragments may have any different shapes or forms, including semi-solid or solid separate parts, fragments, particles, flakes or mixtures thereof. In various implementations, fragments of the film have a recognizable shape. In some implementations, the movie fragment is not accidental. Such shapes include simple geometric forms such as polygons, elliptical forms, triangles, quadrangles (such as a square, rectangle, rhombus), pentagons, hexagons, ovals, circles or shapes that depict figures, animate or inanimate objects such as stars, hearts, pearls, flowers, trees, clovers, letters, numbers, animals, people and the like.

[0084] In addition, multiple film fragments may be in a variety of arrangements, for example, having a first plurality of film fragments in a first color and a second plurality of film fragments in a second color, wherein the first color is different from the second color. Any repositioning of the different compositions is assumed, for example, any number of different active ingredients in the compositions, or different film compositions.

[0085] In some embodiments, the films of the invention can be made using conventional extrusion, blow molding or solution molding processes or other similar methods well known to those skilled in the art. For example, for making a film by a dip molding method, the film-forming polymer is soluble or is dissolved in a sufficient amount of solvent that is compatible with the polymer. Examples of suitable solvents include water, alcohol, acetone, ethyl acetate and mixtures thereof.

[0086] In some embodiments, the film is formed from a solution . Examples of suitable solvents include water, alcohols, acetone, ethyl acetate and mixtures thereof. In one embodiment, the solution comprises a low molecular weight alcohol solvent such as ethanol. After pouring the slurry, the layer is dried to a preferred thickness from about 0.5 mils (13 μm) to about 2 mils (50 μm), although a wider range of thicknesses is feasible and acceptable in the invention.

[0087] After reconstitution, a plasticizer can be added while mixing, and heat can be used if desired to facilitate dissolution until a clear and homogeneous solution is obtained, followed by the addition of abrasives and any other additional ingredients such as thickeners, plasticizers , surfactants, fragrances and / or sweeteners. The solution can cover the appropriate carrier substrate material and dry to form a film. This substrate preferably has a surface tension that allows the polymer solution to be evenly distributed over the entire intended width of this substrate, without soaking, resulting in an unacceptably strong bond between the two substrates. Examples of suitable substrate materials include glass, stainless steel, PTFE commercially available as TEFLON® (DuPont, Wilmington, DE), polyethylene impregnated wrapping paper or polyester liners.

[0088] The film may be dried in an air bath at a moderate to high temperature using a dryer, drying tunnel, vacuum dryer or any other suitable drying equipment that does not adversely affect the active ingredient (s) or the smell of the film. During drying, the films can be subjected to preferential stretching or other orientation processes, such as blowing air along a specific axis of the film to align abrasive particles so that they have the desired orientation in this film. The shaping of the dry film into fragments or shapes in the final form can be carried out by cutting with a blade or using rotary nozzles or in a press with punching dies. Optionally, the carrier substrate may have foundry molds formed in it and the suspension will dry in these molds to the shape determined by the shape of the mold. In some embodiments of the invention, brittle active ingredients can be incorporated into the film composition without affecting or neglecting certain aspects of film production, thereby enabling easier, more economical, and more robust film production.

[0089] Conventional ingredients known to those skilled in the art can be used to prepare the carriers for the compositions described above. The specific composition of the carrier preferably depends on the purpose of the composition. The carrier may be a liquid, semi-solid or solid phase. If the compositions are oral care compositions or personal care compositions, they are preferably provided in a carrier or vehicle acceptable for use in the oral cavity or in dermatology (e.g. in cosmetics). Oral care compositions may be in the form of dentifrices (including toothpastes, tooth gels, mouthwash, tooth powders and preventive pastes), confectionery (including gums, balls and chewing products) , film, paint-on varnishes, professional polishing formulations or any other known form in which abrasives are used. Personal care compositions include soaps, bath gels, body washers, exfoliating abrasives (scrub scrubs), lotions, antiperspirants and deodorants, nail care products and the like. Household compositions include powders, pastes, detergents, fabric softeners, cleaners and the like. The choice of specific carrier components depends on the intended product form.

[0090] In some embodiments, the carrier is aqueous and in this case the carrier contains from about 5% to about 95% water. In other embodiments, the carrier is substantially non-aqueous. [0091] It is well known to those skilled in the art that the carriers of these compositions optionally contain other materials, including, for example, surfactants such as surfactants, emulsifiers and foam modulators, viscosity modifiers as well as thickeners, humectants, diluents , fillers, pH modifying agents, dyes, preservatives, solvents and mixtures thereof. It is understood that although the general characteristics of each of the above categories of materials may be different, there may be some common characteristics and each individual material may serve a variety of purposes within two or more categories of materials.

[0092] Suitable surfactants that are practically stable over a wide pH range and are well known to those skilled in the art are anionic, nonionic or amphoteric surfactants, including those described above in the context of film compositions, which are useful at this site.

[0093] In embodiments of the oral care composition in the form of dentifrices, the exemplary carrier is substantially semi-solid or solid. Dentifrices typically contain surfactants, humectants, viscosity modifiers and / or thickeners, abrasives, solvents such as water, fragrances and sweeteners. As known to those skilled in the art, in addition to the components described above, the oral care compositions optionally contain other materials, including, for example, emollients, moisturizers, mouth refreshers and the like. Examples of suitable carriers for oral care compositions are disclosed in US Patent Nos. US 6,699,929 (Boyd et al.), US 6,379,654 (Gebreselassie et al.), And US 4,899,220 (Nabi et al.) .

[0094] In various embodiments, oral care compositions are provided with one component or phase. In other embodiments, the composition includes first and second components that are held separately. Separate maintenance of components only requires that these components be maintained in such a way as to substantially prevent the interaction of one component of this composition with the other component of this composition. In general, a two-component oral care composition is used when one or more incompatible ingredients are present in the composition. For example, if the carrier contains two incompatible active ingredients, it is preferable to keep them separate. Although films containing active ingredients generally provide some degree of separation, there may be some migration of the active ingredient from the film to the carrier and vice versa, and in this case it may be desirable to introduce a completely separated phase. Separation of components can be accomplished by methods known or discovered in the future; they include chemical, physical and mechanical separation means and any combinations thereof. For example, you can combine the first and second incompatible components but keep some components separately by enveloping or encapsulating one or both into a protective film, envelope, capsule, micelle, etc.

[0095] In embodiments directed to the oral care composition in the form of a confectionery, the exemplary carrier is substantially solid or semi-solid. Confectionery carriers are known in the art, and preferably include chewing gum carriers, which generally contain a chewing gum base, one or more plasticizing agents and a sweetener and a flavoring. Examples of suitable confectionery carriers are given in US Patent Nos. 5,833,954 and 5,933,786 (both belonging to Chow et al.) And US 6,770,264 (Stier et al.).

[0096] In some embodiments, the oral care composition is in the form of an edible film, in fragments comprising a transferred portion of the active ingredient dispersed in the film carrier. The film composition may be any of the compositions described above; however, in some implementations, the film fragments preferably have a composition that is different from the film carrier, such that the film fragments are physically and / or chemically distinct from the film carrier. As known to those skilled in the art, preferred film carriers include soluble films or films having a removable substrate. Non-limiting examples of suitable films are found in US patents

In US Pat. Nos. 4,713,243 (Schiraldi et al.), US 6,419,903, US 6,419,906 and US 6,514,833 (all belonging to Xu et al.) And in US Patent Publication No. US 2004/0062724 (Moro and et al.).

[0097] The film carrier may be designed based on selected polymers such that its dissolution rate corresponds to the predefined duration of treatment. Preferably, the dissolution rate of the film carrier is such that the film carrier breaks down or dissolves at a higher rate than the film containing the active ingredient, which allows controlled release of the active ingredient contained in the carrier film (only the transferred active ingredients in this film) and in the film containing the transferred ingredients active. Carrier films can be made from the same film-forming materials as described in the context of the film containing the transferred active ingredient.

[0098] Carrier films may be made by any conventional film formation methods such as those described above. Preferably, the films containing the active ingredient are incorporated into the film after casting from the solution or before extrusion. The thickness of the carrier film is preferably greater than the film fragments containing the active ingredient. A preferred thickness is from about 12.7 μm (0.5 mils) to about 508 μm (20 mils), although a larger thickness range is possible.

[0099] In some embodiments, the composition is in the form of an oral paint-on or nail composition with a non-aqueous carrier. This varnish carrier is a flowing viscous non-aqueous liquid suspension that is applied to a surface, such as teeth or nails, by hand, with a soft applicator. In some embodiments, the oral care lacquer composition comprises an adhesion-enhancing film-forming polymer that is liquid and hydrophilic, such as polyalkylene glycol polymers, e.g. nonionic polymers of ethylene oxide or a nonionic block copolymer of ethylene oxide and propylene oxide (for example, copolymers called Poloxamer). The carrier of this varnish also optionally contains solvents, plasticizers, mass increasing, filling or viscosity modifying agents. Suitable paint-on varnish carriers are described in US Patent Nos. 6,770.266 (Santarpia et al.) And US 6.669.930 (Hoic et al.).

[0100] Carriers for personal care products may come in many different forms, such as, for example, emulsions, including but not limited to oil-in-water emulsions, water-in-oil, water-in-oil-in-water, and oil-in-water-in-silicone. These emulsions can have a wide viscosity range, e.g. from about 100 centipoise to about 200,000 centipoise. Other suitable carriers include anhydrous liquid solvents such as oils (e.g. vegetable and mineral oils), alcohols (e.g. ethanol, isopropanol) and silicones (e.g. dimethicone, cyclomethicone); aqueous monophasic liquid solvents (e.g., water-alcohol solvent systems); and concentrated versions of these anhydrous and water-based monophasic solvents (i.e., in which the viscosity of the solvent was increased to produce a solid or semi-solid product by the addition of appropriate clays, resins, waxes, polymers, salts and the like). As stated above, carriers for personal care compositions often contain emollients, moisturizers or conditioners, which may also form part of the solvent for the carrier. Soaps, gels, bath lotions and the like preferably contain surface-active detergents. Examples of such carriers are described in US Patent No. US 5,480,633 (Simon et al) [0101] Carriers for the composition of household products or household cleaners preferably contain one or more surface-active detergents, detergent forming agents such as sulfates (e.g. sodium sulfate), phosphates (e.g. trisodium phosphate, disodium phosphate), complex phosphates (e.g. tetrasodium pyrophosphate, sodium tripolyphosphate, sodium tetrafosphate, sodium hexametaphosphate), silicates (e.g. sodium silicate, colloidal silicates), carbonates (e.g. sodium carbonate, sodium bicarbonate), bleaching compounds (e.g. sodium hypochlorite, sodium perborate, sodium percarbonate) as well as optionally activators, pH buffering agents, enzymes, conditioning agents, diluents and the like. Exemplary cleaners are described in US Patent Nos. US 6,670,318 (Hokkirigawa et al.), US 5,294,364 (Thomas et al.), US 4,869,842 (Denis et al.), US 3,965,026 (Lancz ).

[0102] The invention is further illustrated by the following non-limiting examples.

Example 1 [0103] A film composition was prepared using the ingredients listed in Table 1 below.

Table I

<td>Ingredients</td><td>% in the composition (calculated on the wet weight)</td><td>Approximate% content in the composition (calculated as dry) weight)</td>

<td>METHYLCELLULOSE® E5</td><td> 10</td><td> 34</td>

<td>METHYLCELLULOSE® E50</td><td> 3</td><td> 10</td>

<td>Menthol</td><td> 4,4</td><td> 15</td>

<td>Corn starch</td><td> 4</td><td> 14</td>

<td>Canella bark oil</td><td> 2,6</td><td> 9</td>

<td>Titanium dioxide</td><td> 1</td><td> 3</td>

<td>TWEEN® 80</td><td> 0,5</td><td> 2</td>

<td>Propylene glycol</td><td> 2</td><td> 7</td>

<td>Water</td><td>as much as you need</td><td> 5</td>

<td>% solids</td><td> 27,5</td><td> -</td>

[0104] Film is formed from an aqueous solution in which the amount of solids can range from 5% to 60%. Particularly in the example in Table 1, the film is poured from a suspension containing about 70% water. The film is wet formed to a thickness of 229 μm (9 mils) on a removable polyethylene-coated paper substrate and dried in a dryer set to 80^aboutC for about 10 minutes. The film contains menthol (for breath freshening and cooling effect). The film does not contain bleaching agent. Shaping ready-made molds from films is possible by simply cutting with a knife or stamps in rotary or impact presses.

Example 2 [0105] A film composition was prepared using the ingredients listed in Table II below as described in Example 1. The film contains menthol but no bleaching agents.

Table II

<td>Ingredients</td><td>% in the composition (calculated on the wet weight)</td><td>Approximate% content in the composition (calculated as dry) weight)</td>

<td>METHYLCELLULOSE® E5</td><td> 4</td><td> 19</td>

<td>METHYLCELLULOSE® E50</td><td> 4</td><td> 19</td>

<td>Menthol</td><td> 4,4</td><td> 22</td>

<td>Canella bark oil</td><td> 2,6</td><td> 13</td>

<td>Titanium dioxide</td><td> 2</td><td> 10</td>

<td>SOLKA-FLOC® 300</td><td> 1,6</td><td> 8</td>

<td>TWEEN® 80</td><td> 0,25</td><td> 1</td>

<td>Glycerine</td><td> 0,25</td><td> 1</td>

<td>triacetin</td><td> 0,25</td><td> 1</td>

<td>Corn starch</td><td> 0,2</td><td> 1</td>

<td>Water</td><td>as much as you need</td><td> 5</td>

<td>% solids</td><td> 19</td><td> -</td>

Example 3 [0106] A film composition was prepared using the ingredients listed in Table II above in accordance with Example 2. Small squares (0.16 cm; 1/16 inch) were cut from the poured film. Using the film composition of Example 2, a two-phase dentifrice composition containing the ingredients of Table III was prepared. The dentifrice consists of the first part (Part A) and the second part (Part B) and each is prepared separately as follows, with reference to Table III:

The active ingredient to be transferred to the film is a whitening agent (hydrogen peroxide). Sodium saccharin, sodium fluoride, tetrasodium pyrophosphate (TSPP), magnesium gluconate and other salts are suspended in water and mixed in a conventional mixing mixer. Skin moisturizers, e.g. glycerin and sorbitol, are added to this aqueous mixture while mixing. Then organic thickeners such as carrageenan, carboxymethylcellulose, GANTREZ® and any polymers are added. The hydrogen peroxide product is added to Part B. The resulting mixture is mixed to form a homogeneous gel phase. This mixture is transferred to a high speed vacuum mixer, where abrasive and inorganic thickeners are added. The mixture is mixed at high speed for a period of 5 to 30 minutes under reduced pressure from about 20 to about 50 mm Hg. The fragrance oil is weighed and added to the mixture. Finally, surfactants such as sodium lauryl sulfate (SLS) or polyethylene glycol (PEG) are charged to the relevant parts in separate mixers. The film flakes from Example 2 are added to Part B of the formulation and mixed. The parts produced are homogeneous, semi-solid extrudable products in the form of a paste or gel.

[0107] Part A and Part B may be prepared in a two-phase vessel having a partition, such as a two-chamber tube container having a polyethylene partition.

Table III

<td>Ingredient</td><td>Part A (weight%)</td><td>Part B (% by weight)</td>

<td>sorbitol</td><td> 27,5</td><td> -</td>

<td>Saccharin sodium</td><td> 0,6</td><td> -</td>

<td>Sodium tetra pyrophosphate</td><td> 1</td><td> -</td>

<td>Titanium dioxide</td><td> 1</td><td> -</td>

<td>Magnesium gluconate</td><td> 0,05</td><td> -</td>

<td>Sodium Fluoride</td><td> 0,243</td><td> -</td>

<td>Polyethylene glycol 600 (PEG 12)</td><td> 2</td><td> 10</td>

<td>CARBOPOL® 974P</td><td> 12</td><td> 2</td>

<td>Xanthan gum</td><td> -</td><td> 0,4</td>

<td>Sodium hydroxide (50%)</td><td> -</td><td> 0,3</td>

<td>Liquid gantrez (13%)</td><td> -</td><td> -</td>

<td>Sodium hydroxide (50%)</td><td> -</td><td> 0,3</td>

<td>Glycerine</td><td> -</td><td> 40</td>

<td>Phosphoric acid (85%)</td><td> 7,7</td><td> 0,1</td>

<td>Hydrogen peroxide (35%)</td><td> -</td><td> 5,7</td>

<td>Cut fragments of the film from Example 2</td><td> -</td><td> 0,5</td>

<td>Sodium tripolyphosphate</td><td> 7</td><td> -</td>

<td>Sodium carboxymethyl cellulose</td><td> 1</td><td> -</td>

<td>Iota carrageenan</td><td> 0,35</td><td> -</td>

<td>Ingredient</td><td>Part A (weight%)</td><td>Part B (% by weight)</td>

<td>SYLODENT 783</td><td> 11</td><td> -</td>

<td>SYLODENT XWA 650 Efficient silica cleaner abrasive</td><td> 10</td><td></td>

<td>ZEODENT® Silica thickening</td><td> 1,4</td><td></td>

<td>ZEODENT® 115</td><td> -</td><td> 0,15</td>

<td>Laponite D</td><td> 0,75</td><td> -</td>

<td>Sodium lauryl sulfate</td><td> 2</td><td> -</td>

<td>Fragrance</td><td> 1</td><td> 1</td>

<td>Butylhydroxyanisole (BHT)</td><td> -</td><td> 0,03</td>

<td>FD&amp;C Blue Dve Blue # 1 (12.5%)</td><td> -</td><td> 0,27</td>

<td>Water</td><td>as much as you need</td><td>as much as you need</td>

[0108] The results of the determination of the hydrogen peroxide level in the strips taken from Part B of Example 3 are given in Table IV, comparatively with the commercially available whitening strip of Comparative Example A, Crest WHITESTRIPS® from Procter and

Gamble Co. (Cincinnati, OH, United States of America). In addition, tone change testing showed that during 10 to 15 treatments, the whitening strips of Example 3 gave similar results for measurements of ΕΕ soiled, not subjected to prophylactic molar cleaning in SPECTROSHADE ™ analysis as in the Comparative Example. Thus, the transfer of an active ingredient by the methods of the invention results in films containing an effective amount of the transferred active ingredient, so that these films are suitable for use in an oral whitening composition.

Table IV

<td>Whitening strip</td><td>% peroxide</td>

<td>Video from example 3</td><td> 1,82</td>

<td>Comparative Example A</td><td> 4,77</td>

Example 4 [0109] A film composition was prepared using the ingredients listed in Table V below, in the same manner as described in Example 3, except that only one phase was produced and that the active ingredient that was to be transferred to the film was non-ionic antibacterial halogenated diphenyl ether (triclosan).

Table V

<td>Ingredient</td><td>% by weight</td>

<td>Sodium carboxymethyl cellulose</td><td> 0,5</td>

<td>Polyethylene glycol 600 (PEG 12)</td><td> 3</td>

<td>sorbitol</td><td> 67</td>

<td>Saccharin sodium</td><td> 0,4</td>

<td>Sodium Fluoride</td><td> 0,24</td>

<td>Pigment</td><td> 0,002</td>

<td>ZEODENT® 113; silica abrasive</td><td> 9</td>

<td>ZEODENT® 165 Thickening silica</td><td> 8</td>

<td>Triclosan</td><td> 0,3</td>

<td>Perfume oil</td><td> 1,2</td>

<td>Sodium lauryl sulfate</td><td> 1,5</td>

<td>Cut fragments of the film from Example 2</td><td> 0,3</td>

<td>Kokami dop ob etaine</td><td> 0,5</td>

<td>Water</td><td>as much as you need</td>

Example 5 [0110] A medium containing glycerin and peroxide as the active ingredient (e.g., aqueous, 35% hydrogen peroxide solution) can be used to transfer the active ingredient to the film. Many different concentrations of active ingredient can be selected.

[0111] Using fragments of the film composition prepared according to Example 2, a medium is prepared using glycerin and hydrogen peroxide, used as Part B in Example 3, above. A 0.5 wt% film is prepared and mixed with glycerin / hydrogen peroxide medium for 1 to 5 minutes. This film-containing medium is then returned to the oral care composition carrier, i.e., mixed with the other components of the Part B composition as described above, and then other ingredients are added.

Example 6 [0112] Using the film composition prepared in Example 2, many different concentrations of medium are prepared according to Table VI. The transfer time is given for

Examples A, B and C. Film strips are immersed and introduced into the medium by mixing. The determined peroxide levels in the strips taken from the medium at different transfer times are given in Table VI. The amount of peroxide transferred in the film indicates that the portion of peroxide transferred to the film can be selected based on the peroxide concentration in this medium and the duration of the transfer. If the peroxide concentration in the medium is relatively high, then the amount of peroxide transferred is also relatively high and the time required for the transfer can be reduced by obtaining the same concentration in the film.

Table VI

<td>Movie</td><td>Glycerine (% by weight)</td><td>Peroxide (% by weight)</td><td>Movie, pieces (% by weight)</td><td>Time transfer (Minutes)</td><td>Peroxide moved for film (weight%)</td>

<td>Example A</td><td> 30</td><td> 5,7</td><td> 0,5</td><td> 30</td><td> 2,9</td>

<td>Example B</td><td> 20</td><td> 5,7</td><td> 0,5</td><td> 20</td><td> 4,3</td>

<td>Example C</td><td> 4,8</td><td> 1,9</td><td> 0,5</td><td> 15</td><td> 5,1</td>

[0113] In various embodiments, the invention provides a fast and effective method of transferring active ingredients to films. In addition, by first preparing the film composition and then introducing the active ingredients into them, these methods are particularly suitable in embodiments in which the active ingredient is fragile or could be damaged by exposure to the conditions desired in the production of the film.

The active ingredients transferred to the film are stable when stored in a carrier containing, for example, incompatible ingredients and surfactants. In addition, the methods of the invention provide an easy and economical process in the manufacturing plant.

[0114] It should be noted that the description and specific examples provided in the disclosure are for illustrative purposes only and do not limit the scope of the present disclosure.