Solid product containing oil pockets
Abstract
FIELD: food industry. ^ SUBSTANCE: invention relates to a solid product containing oil in the form of pockets as well as to a method for production of the said solid product and its application. The solid oily product containing oil in the form of pockets with a 0.1 - 100 mcm diameter, proteins cross-linked at the separation boundary of the said pockets and a polar low-molecular intermediate compound between the separation boundaries of the cross-linked proteins wherein the polar low-molecular intermediate compound is selected from the group consisting of glycerine and sucrose. ^ EFFECT: invention allows to produce a solid oily product without hydrogenisation of the oil used in it. ^ 16 cl, 2 dwg, 4 ex
Term
Projected expiry 14 March 2027.
- Priority
- Filed
- Granted
- Today
- Projected expiry
16 claims: 9 independent, 7 dependent
- 1A solid oil product containing oil in the form of droplets with a diameter of 0.1 to 100 microns, cross-linked proteins at the interface of said droplets and polar low molecular weight intermediate between interfaces crosslinked proteins, wherein the polar, low molecular weight intermediate selected from the group consisting of glycerol and saccharose. 1. Твердый масляный продукт, содержащий масло в виде капель диаметром от 0,1 до 100 мкм, поперечно сшитые белки на границе раздела указанных капель и полярное низкомолекулярное промежуточное соединение между границами раздела поперечно сшитых белков, в котором полярное, низкомолекулярное промежуточное соединение выбирается из группы, состоящей из глицерина и сахарозы. 1. Твердый масляный продукт, содержащий масло в виде капель диаметром от 0,1 до 100 мкм, поперечно сшитые белки на границе раздела указанных капель и полярное низкомолекулярное промежуточное соединение между границами раздела поперечно сшитых белков, в котором полярное, низкомолекулярное промежуточное соединение выбирается из группы, состоящей из глицерина и сахарозы.
- 6A solid oil product according to any one of the preceding claims 1-5, further comprising glutaraldehyde. 6. Твердый масляный продукт по любому из предшествующих пп.1-5, который содержит также глутаральдегид. 6. Твердый масляный продукт по любому из предшествующих пп.1-5, который содержит также глутаральдегид.
- 7A solid oil product according to any one of the preceding claims 1-5, further comprising transglutaminase. 7. Твердый масляный продукт по любому из предшествующих пп.1-5, который содержит также трансглутаминазу. 7. Твердый масляный продукт по любому из предшествующих пп.1-5, который содержит также трансглутаминазу.
- 8A solid oil product according to any one of the preceding claims 1-5, wherein the amount of protein is from 0.1 to 5 wt.%. 8. Твердый масляный продукт по любому из предшествующих пп.1-5, в котором количество белка составляет от 0,1 до 5 мас.%. 8. Твердый масляный продукт по любому из предшествующих пп.1-5, в котором количество белка составляет от 0,1 до 5 мас.%.
- 9A solid oil product according to any one of the preceding claims 1-5, wherein the amount of polar, low-molecular weight intermediate compounds is up to 2%. 9. Твердый масляный продукт по любому из предшествующих пп.1-5, в котором количество полярного, низкомолекулярного промежуточного соединения составляет до 2%. 9. Твердый масляный продукт по любому из предшествующих пп.1-5, в котором количество полярного, низкомолекулярного промежуточного соединения составляет до 2%.
- 10The method of manufacturing the solid oil product according to any of claims 1-9, wherein:- the oil is dispersed in a protein solution to form an emulsion, - the emulsion is homogenised and washed with water, - glutaraldehyde or transglutaminase is added or the concentrated emulsion is heat treated, and - add a polar, low molecular weight intermediate, which is selected from the group consisting of glycerol and saccharose. 10. Способ производства твердого масляного продукта по любому из пп.1-9, в котором:- масло диспергируют в белковом растворе до образования эмульсии,- эмульсию гомогенизируют и промывают водой,- добавляют глутаральдегид или трансглутаминазу, либо концентрированную эмульсию подвергают тепловой обработке, и- добавляют полярное, низкомолекулярное промежуточное соединение, которое выбирают из группы, состоящей из глицерина и сахарозы. 10. Способ производства твердого масляного продукта по любому из пп.1-9, в котором:- масло диспергируют в белковом растворе до образования эмульсии,- эмульсию гомогенизируют и промывают водой,- добавляют глутаральдегид или трансглутаминазу, либо концентрированную эмульсию подвергают тепловой обработке, и- добавляют полярное, низкомолекулярное промежуточное соединение, которое выбирают из группы, состоящей из глицерина и сахарозы.
- 14Use of the solid oil product according to any of claims 1-9 as an inclusion or matrix in food products, in which to enter non-hydrogenated solidified oil. 14. Применение твердого масляного продукта по любому из пп.1-9 в качестве включения или матрицы в пищевых продуктах, в которые требуется ввести негидрогенизированное отвержденное масло. 14. Применение твердого масляного продукта по любому из пп.1-9 в качестве включения или матрицы в пищевых продуктах, в которые требуется ввести негидрогенизированное отвержденное масло.
- 15Use of the solid oil product according to any of claims 1-9, wherein said solid oil is used in cosmetic products as a solid encapsulating matrix for lipophilic compounds. 15. Применение твердого масляного продукта по любому из пп.1-9, в котором указанное твердое масло используется в косметических изделиях в качестве твердой инкапсулирующей матрицы для липофильных соединений. 15. Применение твердого масляного продукта по любому из пп.1-9, в котором указанное твердое масло используется в косметических изделиях в качестве твердой инкапсулирующей матрицы для липофильных соединений.
- 16Use of the solid oil product according to any of claims 1-9, as a means of low viscosity and lubricity. 16. Применение твердого масляного продукта по любому из пп.1-9, в качестве средства с низкой вязкостно-смазывающей способностью. 16. Применение твердого масляного продукта по любому из пп.1-9, в качестве средства с низкой вязкостно-смазывающей способностью.
Independent claims9
51 paragraphs, as filed
The invention concerns a solid product comprising oil in the form of droplets, and a method of production of said solid product and its use.
Solid oil-based products are already known on the market. An example is margarine. A disadvantage of the margarine is that the oil used to manufacture this product is hydrogenated, which leads to the saturation of the double carbon bonds. Currently, nutrition is known that it is better not to hold and maintain the hydrogenation of unsaturated double bonds, as unsaturation of the double bonds in the oil has beneficial effects on the health of the consumer.
The present invention is a method for manufacturing the solid oil product without hydrogenating the oil used therein.
The present invention concerns a solid product comprising oil in the form of droplets with a diameter of 0.1 to 100 microns, cross-linked proteins at the interface of said droplets and polar low molecular compound demarcations between crosslinked proteins.
As used herein, the term "oil as droplets" means spherical, mainly particles, such polyhedral (polyhedral) particles.
The droplet size distribution is measured by light scattering using a Malvern MasterSizer instrument.
The oil used in the invention is selected from the group consisting of triglycerides and hydrocarbon oils.
More preferably, the oil used is selected from the group consisting of medium chain triglycerides (MCT), olive oil, sunflower oil, paraffin oil and mineral oil.
The protein used in the invention is selected from the group consisting of milk proteins and soy proteins. More preferably, the product of the invention are used β-casein and β-lactoglobulin. It can be used as sodium caseinate.
Low molecular weight intermediate selected from the group consisting of glycerol and saccharose.
The variant in which the solid product of the invention contains glutaraldehyde or transglutaminase. But this option is not the preferred embodiment of the invention.
The amount of oil is from 90 to 100%. In the present description, all% are given as% by weight (wt.%). The amount of protein is from 0.1 to 5%. The amount of low molecular weight intermediate compound is up to 2%.
The present invention also relates to a method for manufacturing the solid oil product as described above, wherein
- Oil is dispersed in a protein solution to yield an emulsion,
- The emulsion is homogenised and washed with water,
- Glutaraldehyde or transglutaminase is added or the concentrated emulsion is subjected to a heat treatment and
- Added a polar low-molecular intermediate.
According to a preferred embodiment of the invention, the heat treatment is carried out under emulsion temperature of about 80 ° C for about 10 to 60 minutes in the absence of enzymatic or chemical crosslinking agents.
According to a second embodiment of the emulsion is poured in the same volume of aqueous 1 wt.% Of glutaraldehyde is maintained for a while and washed to remove unreacted glutaraldehyde.
According to a third embodiment of the emulsion is poured in the same volume of aqueous 1 Transglutaminase unit / g.
The present invention relates to the use of the solid oil product as described above, wherein said solid oil product may be used as inclusion or matrix in food products, in which to enter non-hydrogenated solidified oil. The amount of the solid oil product added in the food product can vary very widely. For example, the amount may be from 0.1 to 99%. The form of the food, which is added in the solid product of the invention is not critical. For example, it can be added in culinary products of any type.
In accordance with another feature of the invention, the product of the invention is used in cosmetic products as a solid encapsulated matrix for lipophilic compounds. In this case, the amount of administered product may also vary widely. It may be from 0.1 to 99%.
In accordance with another feature of the invention, the use of the solid oil product may be due to its low viscosity and lubricity.
The product of the invention may have the property of re-emulsification (in this case, it is good to use for culinary products) or may not have such properties (in this case, it is suitable for use in cosmetic products and in the manufacture of lubricants).
Finally, the present invention relates to a method for producing a solid oil with inhomogeneous cell composition, wherein said solid oil is produced as described above by mixing two different oil emulsions cross-linked as described above, and subjecting the mixture of emulsions evaporate moisture to form a gel whose cells formed on multiple oil phases.
The following description of the invention given with reference to the drawings.
1 shows an internal structure of the gel formed a monodisperse emulsion containing droplets with a diameter of 80 mm, which was able to be detected by confocal microscopy. To obtain an image the protein phase to buffered (pH to 7.0) aqueous phase used in the final washing step was added at a concentration of rhodamine 1010 M.
2 shows the rehydration thermally crosslinked gel based on paraffin oil with R = 0.5 um. The white squares show the droplet radius distribution of emulsion obtained after crosslinking. The black squares show the droplet radius distribution of emulsion obtained after rehydration of the dried gel with 20 mM buffer (pH 7.0) solution of imidazole. Figure 2 shows that the process is fully reversible: the droplet size remains the same as in the initial emulsion.
The polar low molecular compound is detected when re-emulsified in water of a solid product by analyzing the composition of water containing said polar low molecular compound.
The following are examples of the invention.
Example 1.
Preparation of Emulsion
A coarse oil-in-water emulsion in which the dispersed phase has a diameter of 0.5 microns can be obtained by the progressive introduction of MCT (medium chain triglycerides) with continuous stirring in 1 wt.% Protein solution having a pH 7.0. The protein solution may be a buffer solution (20mM imidazole solution, non food-grade method for) or the pH can be set at pH 7.0 by addition of sodium hydroxide (Method for food products).
The resulting coarse emulsion is homogenized for 300 sec using a rotary disperser or a high pressure homogenizer to obtain the smallest size drops. The shearing speed / pressure determines the average droplet size of the emulsion sample and accordingly the average cell size.
The emulsion is maintained for about 1 hour to complete protein adsorption. Further, the emulsion is washed, ie unabsorbed protein in solution is removed by dilution. This is achieved by settling the emulsion in a decanter or in case of thinner emulsions by centrifugation. The aqueous phase is removed and the concentrated emulsion is re-diluted about 5-fold volume of water (Method for food products) or 20 mM imidazole buffer pH 7.0. This step is repeated twice to dilute unadsorbed protein in the continuous phase by two orders of its amount. The above irreversible protein adsorption provides stable emulsions with very low amounts of non-adsorbed proteins. Nonadsorbed protein can be reused.
Example 2.
Preparation of the gel with glutaraldehyde
Adsorbed protein molecules cross-linked to ensure protein layer stability upon subsequent removal of the continuous phase. Crosslinking adsorbed protein is achieved chemically with glutaraldehyde to yield non-edible material.
The concentrated, washed emulsion is poured in the same volume of buffer solution (pH 7.0) 1 wt.% Of glutaraldehyde to provide crosslinking adsorbed protein molecules while preventing crosslinking between the particles. The dilute emulsion is maintained for 5 minutes under gentle stirring. After crosslinking of the unreacted glutaraldehyde was washed out of the emulsion in the same manner as in step 3 (See above.) To obtain a concentrated emulsion with cross-linked proteins at the interface. This method gives non-food material.
Glycerol or D (+) - Saccharose is added to the supernatant concentrated emulsions up to a concentration of 0.5 wt.% Under gentle stirring. The concentrated emulsion is mold into the recipient with a high ratio of width to height and exposed Drain under aeration for 72 hours at room temperature to yield a lipidic transparent gel. Measurement of the diameter of the oil droplets with a Malvern MasterSizer gives showed that the order of 80 microns.
Example 3.
Preparation of a gel with transglutaminase (TGase)
Another way of crosslinking the proteins comprises adding TGase. The concentrated, washed emulsion is poured in the same volume of a solution of 1 u / g TGase and aged for 1 hour under gentle stirring. The emulsion is then washed to separate the unadsorbed TGase and TGase carrier in the same way as in Step 3 (See above.), And kept in a dilute state at 55 ° C for about 10 hours. Being a protein, TGase concurrently and irreversibly adsorbs at the oil-water interface. The washing step ensures that no pH shift of the ground during the 10-hour period at 55 ° C. This method yields a food material.
Glycerol or D (+) - Saccharose is added to the concentrated emulsion-settled to a concentration of 0.5 wt.% Under gentle stirring. The concentrated emulsion is mold into the recipient with a high ratio of width to height and exposed Drain under aeration for 72 hours at room temperature to yield a lipidic transparent gel.
Measurement of the diameter of the oil droplets with a Malvern MasterSizer gives showed that the order of 80 microns.
Example 4.
Preparation of the gel by heat treatment
Another way of crosslinking the proteins involves heat treatment of the emulsion.
The concentrated, washed emulsion is heated in an oven to 80 ° C and maintained at this temperature for 1 hour. This method yields a food material.
Glycerol or D (+) - Saccharose is added in spaced concentrated emulsions up to a concentration of 0.5 wt.% Under gentle stirring. The concentrated emulsion is mold into the recipient with a high ratio of width to height and exposed Drain under ventilation during 72 hours at room temperature to yield a lipidic transparent gel.
Measurement of the diameter of the oil droplets with a Malvern MasterSizer gives showed that the order of 80 microns.
Every citation, both ways
| Document | Relation | Office | Cited during |
|---|---|---|---|
| RU2668396C2 | Cited by | Russian Federation | Search report |
| WO2005110370A1 | Cites | World Intellectual Property Organization (WIPO) | – |
| US5248509A | Cites | United States of America | – |
| US5620734A | Cites | United States of America | – |
30 members in 18 offices
Priority claims5
| Document | Office | Kind | Date |
|---|---|---|---|
| 06111524 | European Patent Office (EPO) | A | |
| 06111524 | European Patent Office (EPO) | A | |
| 061115242 | European Patent Office (EPO) | – | |
| 061115242 | – | – | – |
| EP20060111524 | – | – | – |
Members30
| Document | Office | Kind | |
|---|---|---|---|
| EP1836897A1 | European Patent Office (EPO) | A1 | |
| AU2007228820A1 | Australia | A1 | |
| CA2645584A1 | Canada | A1 | |
| WO2007107490A1 | World Intellectual Property Organization (WIPO) | A1 | |
| NO20083929L | Norway | L | |
| EP1998627A1 | European Patent Office (EPO) | A1 | |
| CN101404890A | China | A | |
| JP2009534016A | Japan | A | |
| EP1998627B1 | European Patent Office (EPO) | B1 | |
| AT447328T | Austria | T | |
| ATE447328T1 | Austria | T1 | |
| US2009304896A1 | United States of America | A1 | |
| DE602007003084D1 | Germany | D1 | |
| PT1998627E | Portugal | E | |
| ES2333179T3 | Spain | T3 | |
| RU2008141779A | Russian Federation | A | |
| PL1998627T3 | Poland | T3 | |
| UA94096C2 | Ukraine | C2 | |
| NZ571090A | New Zealand | A | |
| BRPI0709048A2 | Brazil | A2 | |
| RU2425581C2This record | Russian Federation | C2 | |
| US8147896B2 | United States of America | B2 | |
| US2012189849A1 | United States of America | A1 | |
| AU2007228820B2 | Australia | B2 | |
| JP5107336B2 | Japan | B2 | |
| CN101404890B | China | B | |
| US8668946B2 | United States of America | B2 | |
| CA2645584C | Canada | C | |
| IL193862A | Israel | A | |
| NO337495B1 | Norway | B1 |
4 legal events, as the office reported them to INPADOC
Over the term
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|---|---|---|
| The patent is invalid due to non-payment of feesMM4A | MM4A | |
| Official registration of the transfer of the exclusive right without contract for inventionsPC43 | PC43 | |
| Official registration of the termination of the licence agreement or other agreements on the disposal of an exclusive rightLICENCE FORMERLY AGREED ON 20101006QC41 | QC41 | |
| Official registration of changes to a registered agreement (patent)LICENCE FORMERLY AGREED ON 20101006QZ41 | QZ41 |
Numbers
- Publication
- 2425581
- Publication, DOCDB
- 2425581
- Publication, EPODOC
- RU2425581
- Application
- 200814177913
- Application, DOCDB
- 2008141779
- Application, EPODOC
- RU20080141779
Titles3
- Russian
- ТВЕРДЫЙ ПРОДУКТ, СОДЕРЖАЩИЙ КАПЛИ МАСЛА
- English
- SOLID PRODUCT CONTAINING OIL POCKETS
- Russian
- ??????? ???????, ?????????? ????? ?????
Classification
- CPC, 5
- A23D7/02
- A23D7/0053
- A23D7/0056
- A23L29/10
- Y10T428/2982
- IPC, 5
- A23D7 00
- A23D7 05
- A23L21 10
- A23L29 10
- A23L29 206