CN113440467A

CN113440467A - Repairing and moistening hydrogel microcapsule containing donkey-hide gelatin as well as preparation method and application of repairing and moistening hydrogel microcapsule

Info

Publication number: CN113440467A
Application number: CN202110615477.0A
Authority: CN
Inventors: 廖峰; 樊雨梅; 段平超; 严泽民; 袁彦洁; 赵海晴; 高登锋
Original assignee: Dong E E Jiao Co Ltd
Current assignee: Dong E E Jiao Co Ltd
Priority date: 2021-06-02
Filing date: 2021-06-02
Publication date: 2021-09-28
Anticipated expiration: 2041-06-02
Also published as: CN113440467B

Abstract

The invention discloses a repairing and moistening hydrogel microcapsule containing donkey-hide gelatin, a preparation method and an application thereof, wherein the repairing and moistening hydrogel microcapsule comprises: the repairing and moistening hydrogel microcapsule comprises a capsule core and a capsule wall, wherein the capsule wall is coated outside the capsule core, the average particle size of the repairing and moistening hydrogel microcapsule is 0.5-4mm, and the ratio of the capsule core to the capsule wall is 1: 1-3; the capsule wall contains calcium alginate, agar, phenoxyethanol, caprylic/capric triglyceride, p-hydroxyacetophenone and water; the capsule core contains lactobacillus/rice fermentation product lysate, schizosaccharomyces fermentation product lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, p-hydroxyacetophenone, polysorbate-20, xanthan gum, glycerol, butanediol and water, and the capsule overcomes the defect that the use of the donkey-hide gelatin in the prior art is limited in the cosmetic.

Description

Repairing and moistening hydrogel microcapsule containing donkey-hide gelatin as well as preparation method and application of repairing and moistening hydrogel microcapsule

Technical Field

The invention relates to the field of donkey-hide gelatin cosmetics, in particular to a repairing and moistening hydrogel microcapsule containing donkey-hide gelatin and a preparation method and application thereof.

Background

With the improvement of living standard and the coming of aging society, the public has stronger and stronger consciousness on beauty, and has attracted wide attention to the aging delay. Collagen and hydrolysate thereof have good biological activity, permeability and skin repair capacity, and the application of the collagen and the hydrolysate thereof in the aspect of skin protection is receiving more and more attention. The research has proved that the collagen and the hydrolysate thereof can effectively repair endogenous collagen and elastin fiber, reduce the degradation of extracellular matrix, increase the content of the collagen and realize the effect of delaying senility.

The main active ingredient of colla Corii Asini is collagen and its hydrolysate. Modern pharmacological research results show that the donkey-hide gelatin has the effects of resisting oxidation and aging and repairing skin barriers. At present, the application mode of the donkey-hide gelatin in cosmetics is mainly to prepare donkey-hide gelatin powder to be directly added into the cosmetics. However, in the traditional formula, the direct addition of bioactive ingredients can affect the material properties, bioactivity, etc. of the product; more importantly: the donkey-hide gelatin powder has the characteristics of high viscosity, easiness in moisture absorption and agglomeration, poor solubility and unique gelatin fragrance, so that the use of the donkey-hide gelatin powder in a cosmetic formula is limited.

The microcapsule granulation technology is a technology for embedding and sealing solid, liquid or gas in a microcapsule to form a solid particle product, and the microcapsule technology can improve color, control release, enhance stability, cover bad flavor and prevent reaction among materials. In view of the above-mentioned drawbacks of donkey-hide gelatin, patent document No. CN107050055A discloses a microcapsule skin softening film of donkey-hide gelatin, which comprises: the donkey-hide gelatin is cooled to-50 to-60 ℃ by dry ice, the cooled donkey-hide gelatin is mixed with the dry ice with equal mass, and then the mixture is crushed to particles with the size of 0.1 to 0.5mm in a low-speed crusher; mixing the crushed low-temperature donkey-hide gelatin powder with dry ice with the mass of three times, and quickly crushing for 1min to obtain mixed powder of donkey-hide gelatin and dry ice; dissolving a surfactant, an anionic high-molecular emulsion stabilizer and glycerol in olive oil to prepare a fatty solution, and adding the fatty solution into the mixed powder obtained in the step (2) to obtain core material powder; adding the core powder obtained in the step (3) into sterilized distilled water in batches, controlling the temperature to be 20-35 ℃, and stirring for 3 hours to obtain an emulsion; adding 1 wt% of citric acid into the emulsion obtained in the step (4), adjusting the pH of the emulsion to 4.5, stirring at 40-60 ℃ for 8-10 h, and finally adjusting the pH to 7 by using 1 wt% of sodium bicarbonate solution to obtain a microcapsule dispersion liquid; and (3) soaking the polypropylene non-woven fabric with the thickness of 2-5 mm in the microcapsule dispersion liquid, and taking out to obtain the donkey-hide gelatin microcapsule skin softening film.

Although the scheme can solve the defect of limited use of the donkey-hide gelatin in cosmetics to a certain extent, the method still has the following defects: 1) the scheme uses dry ice, the melting point of the dry ice is-78.5 ℃, low-temperature burn is easily caused in the using process, and meanwhile, the use of the dry ice increases the production cost; 2) in the scheme, the microcapsules are prepared by adopting an emulsification mode, so that the microcapsules have poor stability and are easy to demulsify, and collagen and hydrolysate thereof cannot be continuously and stably absorbed by skin; 3) in the scheme, the polypropylene non-woven fabric is required to load the microcapsule dispersion liquid, and in cosmetics, the variety of the non-woven fabric is very few, so that the application range of the donkey-hide gelatin is further limited; 4) the product prepared by the method has single function, can only improve the keratinization phenomenon of the skin, and cannot carry out deep care on the skin.

Disclosure of Invention

The invention aims to provide a repairing and moistening hydrogel microcapsule containing donkey-hide gelatin and a preparation method and application thereof, so as to overcome the defect that the use of the donkey-hide gelatin in cosmetics is limited in the prior art.

In order to achieve the above object, the present invention provides a repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin, comprising: the repairing and moistening hydrogel microcapsule comprises a capsule core and a capsule wall, wherein the capsule wall is coated outside the capsule core, the average particle size of the repairing and moistening hydrogel microcapsule is 0.5-4mm, and the diameter ratio of the capsule core to the capsule wall is 1: 1-3;

the capsule wall comprises the following components in percentage by weight of 1: 0.5-4.0: 0.25-1.2: 0.25-2.0: 15-35: 60-80 parts of calcium alginate, agar, phenoxyethanol, p-hydroxyacetophenone, caprylic/capric triglyceride and water;

the capsule core comprises the following components in percentage by weight of 1: 0.1-1.5: 0.1-1.5: 0.1-1.5: 0.1-1.5: 1.0-10: 0.08-1.5: 0.08-1.5: 0.08-1.5: 1.0-12: 1.0-12: 2.0-10: 60-90 of a split yeast fermentation lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butylene glycol, water, and a lactic acid bacteria/rice fermentation lysate.

The invention also provides a preparation method of the repairing and moistening hydrogel microcapsule containing donkey-hide gelatin, which comprises the following steps:

1) mixing the components in a weight ratio of 1: 0.5-4.0: 0.25-1.2: 0.25-2.0: 15-35: mixing 60-80 parts of calcium alginate, agar, phenoxyethanol, p-hydroxyacetophenone, caprylic/capric triglyceride and water to obtain a capsule wall mixed solution;

2) mixing the components in a weight ratio of 1: 0.1-1.5: 0.1-1.5: 0.1-1.5: 0.1-1.5: 1.0-10: 0.08-1.5: 0.08-1.5: 0.08-1.5: 1.0-12: 1.0-12: 2.0-10: mixing 60-90 of split yeast fermentation product lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, colla Corii Asini, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butanediol, water, and lactobacillus/rice fermentation product lysate, heating to 45-65 deg.C, and homogenizing under 45-55MPa for 3-10min to obtain capsule core mixture;

3) coating the capsule wall mixed solution outside the capsule core mixed solution by a dripping method to prepare the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin, wherein the average particle size of the repairing and moistening hydrogel microcapsule is 0.5-4mm, and the diameter ratio of the capsule core to the capsule wall is 1: 1-3.

The invention further provides an application of the repairing and moistening hydrogel microcapsule containing donkey-hide gelatin in preparation of anti-aging cosmetics.

In the technical scheme, the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin is spherical, and the capsule core is semitransparent. In the capsule core, the donkey-hide gelatin can be uniformly dispersed in the capsule core mixed solution under the synergistic action of butanediol, glycerol and polysorbate-20, so that the defects of high donkey-hide gelatin viscosity and easy caking are effectively overcome.

Meanwhile, the lactobacillus/rice fermentation product lysate has the function of improving the skin barrier; the lysate of the yeast fermentation product of the second split can condition the microbial ecological environment of the skin and repair and maintain the skin stably; the acetyl hexapeptide-8 can effectively prevent and relieve the phenomenon of dynamic wrinkles caused by repeated folding of the skin; the palmitoyl tripeptide-1 and palmitoyl tetrapeptide-7 can accelerate the collagen production speed of dermal cells and effectively improve wrinkles; the xanthan gum can relieve dry skin, resist oxidation and remove wrinkles; the p-hydroxyacetophenone has the effects of promoting the preservative effect, resisting oxidation and stimulation and protecting the stability of the emulsion; the 1, 2-hexanediol has the functions of moisturizing and resisting oxidation; the glycerin can supplement water, preserve moisture and lock water. Under the action of the components, the donkey-hide gelatin and the components form compatibility, so that the capsule core can continuously and stably repair skin which is easily damaged by the external environment after being released through the capsule wall, and prevent light damage and photoaging, thereby playing a role in resisting aging. More importantly, the proportion of each component in the capsule core is obtained by creative labor of the applicant, so that the capsule core can play the optimal anti-aging role.

Further, the inventors found, through creative work: the type and thickness of the capsule wall material have a significant influence on the release rate of the capsule core, and the excessive release rate causes the components of the capsule core not to be completely absorbed by the skin, so that most of the nutrient components are lost; and the slow release rate causes the skin care product to be washed and removed when the nutritional components in the capsule core are not completely released. In the invention, calcium alginate, agar, p-hydroxyacetophenone, caprylic/capric triglyceride are used as adhesives, and phenoxyethanol is used as a preservative, so that the embedding effect of the capsule wall is good, the embedding rate is up to 91.36%, and the activity of the compound components in the capsule core can be effectively protected from losing during the storage period. In addition, the proportion of the components in the capsule wall and the thicknesses of the capsule core and the capsule wall are also creatively obtained by the inventor, and the controlled capsule core can be stably released through the capsule wall.

On the basis, the preparation method adopts a heat treatment and homogenization mode to ensure that all components in the capsule core can be mutually dispersed, so that the phenomenon of donkey-hide gelatin agglomeration is effectively avoided; on the other hand, the repairing and moistening hydrogel microcapsule prepared by adopting a dripping method is more stable in structure and is not easy to break emulsion.

It can be seen that the present invention has at least the following advantages compared to the prior art: 1) under the synergistic effect of butanediol, glycerol and polysorbate-20, colla Corii Asini can be stably dispersed in capsule core by heat treatment and homogenization, and is not easy to adhere, so that effective components in colla Corii Asini can be absorbed by skin; and the use of dry ice in the prior art is avoided, so that the production cost is reduced, and the operation safety can be improved.

2) Compared with the prior art which singly improves the keratinization of the skin, the existence of other components such as lactobacillus/rice fermentation product lysate, yeast dehiscence product lysate and the like in the invention forms compatibility with the donkey-hide gelatin, can deeply repair and moisturize the skin, effectively regulate the barrier function of the skin, improve the immunologic function of the skin and help the skin to resist the pressure and the influence from the environment.

3) According to the invention, the capsule wall mixed liquid prepared from specific components is coated outside the capsule core mixed liquid by a dripping method, so that the capsule wall outside the capsule core is more stable, and the demulsification phenomenon is effectively avoided.

4) The use of calcium alginate and agar enables the repairing and moistening hydrogel microcapsule containing donkey-hide gelatin to be dispersed in most cosmetic systems, thereby effectively improving the application range of the repairing and moistening hydrogel microcapsule and avoiding the defect that the microcapsule in the prior art only adopts non-woven fabrics as a carrier.

Additional features and advantages of the invention will be set forth in the detailed description which follows.

Detailed Description

The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.

The invention provides a repairing and moistening hydrogel microcapsule containing donkey-hide gelatin, which comprises the following components in part by weight: the repairing and moistening hydrogel microcapsule comprises a capsule core and a capsule wall, wherein the capsule wall is coated outside the capsule core, the average particle size of the repairing and moistening hydrogel microcapsule is 0.5-4mm, and the diameter ratio of the capsule core to the capsule wall is 1: 1-3;

the capsule core comprises the following components in percentage by weight of 1: 0.1-1.5: 0.1-1.5: 0.1-1.5: 0.1-1.5: 1.0-10: 0.08-1.5: 0.08-1.5: 0.08-1.5: 1.0-12: 1.0-12: 2.0-10: 60-90 of a split yeast fermentation lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butylene glycol, water, lactic acid bacteria/rice fermentation lysate.

In the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin provided by the invention, the content of each component of the capsule wall can be selected in a wide range, but in order to further improve the embedding effect of the capsule wall and the release effect of the capsule core, the weight ratio of the calcium alginate, the agar, the phenoxyethanol, the p-hydroxyacetophenone, the caprylic/capric triglyceride and the water is preferably 1: 1.0-2.0: 1.0-1.2: 1.0-2.0: 20-30: 65-75.

In the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin provided by the invention, the content of each component of the capsule core can be selected in a wide range, but in order to further improve the repairing and anti-aging effects of the capsule core on skin, preferably, the weight ratio of the schizosaccharomyces cerevisiae fermentation product lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butanediol, water, lactobacillus/rice fermentation product lysate is 1: 0.1-1.0: 0.1-1.0: 0.1-1.0: 0.1-1.0: 2-8: 0.08-1.0: 0.08-1.0: 0.08-1.0: 2-8.0: 2-8.0: 2-6.0: 70-90.

In the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin provided by the invention, the size of the capsule core and the size and weight of the capsule wall can be selected in a wide range, but in order to further improve the repairing and anti-aging effects of the capsule core on skin, preferably, the repairing and moisturizing hydrogel microcapsule has the average particle size of 1-3mm, and the diameter ratio of the capsule core to the capsule wall is 1: 1.5-2.5.

In the present invention, in order to further improve the color of the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin, preferably, the capsule wall further contains a coloring agent, and the coloring agent contains CI 77019 (the ingredient is mica) and CI77891 (the ingredient is TiO)₂) CI77491 (the component is iron oxide red); the weight ratio of the calcium alginate to the CI 77019 to the CI77891 to the CI77491 is 1:0.1-0.3：0.1-0.3：0.05-0.15。

Wherein, the dropping method comprises the following operations: and (3) allowing the capsule wall mixed liquid to flow out of the dripper, allowing the homogenized capsule core mixed liquid to flow out of the dripper to form a sandwiched liquid column, and cutting off the liquid column with a cutter to form a series of liquid drops, namely hydrogel microcapsules.

In the above preparation method, the amount of each component in the capsule wall mixture can be selected within a wide range, but in order to further enhance the effect of improving the encapsulation of the capsule wall and the release effect of the capsule core, it is preferable that the weight ratio of the calcium alginate, agar, phenoxyethanol, p-hydroxyacetophenone, caprylic/capric triglyceride and water is 1: 1.0-2.0: 1.0-1.2: 1.0-2.0: 20-30: 65-75.

In the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin provided by the invention, the dosage of each component of the capsule core can be selected in a wide range, but in order to further improve the repairing and anti-aging effects of the capsule core on skin, preferably, the weight ratio of the schizosaccharomyces cerevisiae fermentation product lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butanediol, water, lactobacillus/rice fermentation product lysate is 1: 0.1-1.0: 0.1-1.0: 0.1-1.0: 0.1-1.0: 2-8: 0.08-1.0: 0.08-1.0: 0.08-1.0: 2-8.0: 2-8.0: 2-6.0: 70-90.

In the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin provided by the invention, the size of the capsule core and the size and weight of the capsule wall can be selected in a wide range, but in order to further improve the repairing and anti-aging effects of the capsule core on skin, preferably, in the step 1), the average particle size of the repairing and moisturizing hydrogel microcapsule is 1-3mm, and the diameter ratio of the capsule core to the capsule wall is 1: 1.5-2.5.

In step 1) of the present invention, the mixing temperature can be selected within a wide range, but in order to more uniformly disperse the gelatin in the capsule-core mixture, it is preferable that the mixing is performed at 70 to 80 ℃ in step 1).

In step 2) of the present invention, the heating manner can be selected within a wide range, but in order to more uniformly disperse the donkey-hide gelatin in the capsule-core mixed solution, it is preferable that, in step 2), the system is heated from 15 to 25 ℃ to 45 to 65 ℃ at a heating rate of 0.1 to 0.3 ℃/min after the completion of the mixing.

In step 2) of the present invention, the homogenization method can be selected within a wide range, and can be performed in one step, or in multiple steps, but in order to more uniformly disperse the donkey-hide gelatin in the capsule-core mixed solution, preferably, in step 2), the homogenization treatment is performed in a stepwise manner, and includes a first homogenization and a second homogenization which are sequentially and continuously performed, wherein the first homogenization pressure is 45-50MPa, the second homogenization pressure is 51-55MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.2-0.5.

In the present invention, in order to further improve the color of the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin, preferably, in step 1), CI 77019, CI77891, CI77491, calcium alginate, agar, phenoxyethanol, p-hydroxyacetophenone, caprylic/capric triglyceride and water are mixed to obtain a capsule wall mixed solution; the weight ratio of the calcium alginate to the CI 77019 to the CI77891 to the CI77491 is 1: 0.1-0.3: 0.1-0.3: 0.05-0.15.

In the above application, the addition amount of the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin may be selected in a wide range, but from the viewpoint of skin care effect and cost, it is preferable that the addition amount of the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin is 0.1 to 8% by weight in the anti-aging cosmetic.

In the above-mentioned applications, the kind of the anti-aging cosmetic may also be selected from a wide range, but the anti-aging cosmetic is an anti-aging eye cream type cosmetic or a face cream type cosmetic in view of the range of use of the anti-aging cosmetic.

The present invention will be described in detail below by way of examples. In the case of the examples described below, the,

phenoxyethanol is a commercial product with the batch number of 20210106 of Beijing Sangpu biochemistry technology Limited company;

p-hydroxyacetophenone is a commercially available product with batch number 20200111-2 from Smyris company;

the lactobacillus/rice fermentation lysate is a commercial product with a batch number of 20200828F290DM from Beijing science and technology Limited;

the split yeast fermentation lysate is a commercially available product of Chemisches laboratory rium Dr. Kurt Richter Gmbh company, batch No. 3196412;

the acetyl hexapeptide-8 is a commercial product with the batch number of DC045200801 of Shenzhen Reddlin science and technology Limited;

the palmitoyl tripeptide-1 is a product sold in Shenzhen Shendelin science and technology Limited under the batch number of 147732-56-7;

palmitoyl tetrapeptide-7 is a commercial product with a batch number of 221227-05-0 of Shenzhen Reddlin science and technology Limited;

the colla Corii Asini is a commercial product of Dong' e colla Corii Asini GmbH with a lot number of 2004004;

polysorbate-20 is commercially available from lonza under the trade designation H9415129;

1,2 hexanediol is a commercial product with the batch number CZ9L183-2112 of the THOR company;

xanthan gum is commercially available from CP Kelco under the trade designation 9L 9165K;

glycerol is a commercially available product with a batch number of 2719LME3L from PT Musim Mas;

butanediol is commercially available from Daicel Corporation under the trade designation 13 bgc-jk-061;

the caprylic/capric triglyceride is a commercial product of IOI Esterchem (M) Sdn Bhd company with the batch number MCT6D1031, and the density is 0.95 g/mL;

CI77491 is a commercial product sold under lot number 20200320 by PIGMENT FOR XENSHANZHUJU, Guangzhou.

Example 1

1) The capsule wall material comprises 10g of calcium alginate, 20g of agar, 778913 g of CI, 770193 g of CI, 911.5 g of CI774911, 12g of phenoxyethanol, 20g of p-hydroxyacetophenone and 280.5g of caprylic/capric triglyceride. The capsule wall material is added into 650mL of deionized water, heated and stirred uniformly at 75 ℃ to obtain a capsule wall mixed solution.

2) The capsule core material comprises 700g of lactobacillus/rice fermentation product, 10g of schizosaccharomyces cerevisiae fermentation product lysate, 10g of acetyl hexapeptide-8, 10g of palmitoyl tripeptide-1, 10g of palmitoyl tetrapeptide-7, 80g of donkey-hide gelatin, 10g of polysorbate-20, 10g of xanthan gum, 10g of 1, 2-hexanediol, 10g of p-hydroxyacetophenone, 50g of glycerol, 50g of butanediol and 40mL of water.

Mixing capsule core materials, heating to 50 ℃ from 25 ℃ at a heating rate of 0.2 ℃/min, uniformly stirring, and homogenizing for 3min (wherein, the homogenization comprises a first homogenization and a second homogenization which are sequentially and continuously carried out, the homogenization pressure of the first homogenization is 48MPa, the homogenization pressure of the second homogenization is 52MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.3), so as to prepare a capsule core mixed solution.

3) Preparing hydrogel microcapsules by a dripping method, allowing uniformly stirred capsule wall mixed liquor to flow out of a dripper, allowing well homogenized capsule core mixed liquor to flow out of the dripper to form a sandwiched liquid column, and cutting off the liquid column by a cutter to form a series of hydrogel microcapsules with the diameter of 3mm and the diameter ratio of capsule core to capsule wall of 1: 2 to prepare hydrogel microcapsules. The repairing and moistening hydrogel microcapsule is pearl-shaped spherical, the capsule wall is yellow and semitransparent, and the capsule core is semitransparent.

The formula for calculating the embedding rate is as follows:

wherein Q represents an encapsulation efficiency, W_{General assembly}Represents the total amount of donkey-hide gelatin charged; w_{Swimming device}Indicating the amount of gum that was not encapsulated in the microcapsules.

Under the condition, the embedding rate of the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin is up to 94.39 percent, which shows that the capsule wall has good embedding effect on the capsule core and can effectively prevent the activity of natural compound ingredients from losing during storage.

Example 2

1) The capsule wall material comprises 10g of calcium alginate, 10g of agar, 778911 g of CI, 770191 g of CI, 774910.5 g of CI, 10g of phenoxyethanol, 10g of p-hydroxyacetophenone and 207.5g of caprylic/capric triglyceride. The capsule wall material is added into 750mL deionized water, heated and stirred uniformly at 70 ℃ to obtain a capsule wall mixed solution.

2) The capsule core material comprises 900g of lactobacillus/rice fermentation product, 10g of schizosaccharomyces cerevisiae fermentation product lysate, 1g of acetyl hexapeptide-8, 1g of palmitoyl tripeptide-1, 1g of palmitoyl tetrapeptide-7, 20g of donkey-hide gelatin, 2g of polysorbate-20, 2g of xanthan gum, 1, 2-hexanediol, 2g of p-hydroxyacetophenone, 20g of glycerol, 20g of butanediol and 20mL of water.

Mixing the capsule core materials, heating to 50 ℃ from 15 ℃ at a heating rate of 0.3 ℃/min, uniformly stirring, and homogenizing for 5min (wherein, the homogenization comprises a first homogenization and a second homogenization which are sequentially and continuously carried out, the homogenization pressure of the first homogenization is 45MPa, the homogenization pressure of the second homogenization is 55MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.2), so as to prepare the capsule core mixed solution.

The formula for calculating the embedding rate is as follows:

Under the condition, the embedding rate of the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin is as high as 93.66 percent, which shows that the capsule wall has good embedding effect on the capsule core and can effectively prevent the activity of natural compound components from losing during the storage period.

Example 3

1) The capsule wall material comprises 10g of calcium alginate, 15g of agar, CI 778912 g, CI 770192 g and CI 774911 g, 10g of phenoxyethanol, 15g of p-hydroxyacetophenone and 245g of caprylic/capric triglyceride. The capsule wall material is added into 700mL deionized water, heated and stirred uniformly at 80 ℃ to obtain capsule wall mixed liquid.

2) The capsule core material comprises 720g of lactobacillus/rice fermentation product, 10g of schizosaccharomyces cerevisiae fermentation product lysate, 5g of acetyl hexapeptide-8, 5g of palmitoyl tripeptide-1, 5g of palmitoyl tetrapeptide-7, 47.6g of donkey-hide gelatin, 0.8g of polysorbate-20, 0.8g of xanthan gum, 5g of 1, 2-hexanediol, 0.8g of p-hydroxyacetophenone, 70g of glycerol, 70g of butanediol and 60mL of water. Mixing the capsule core materials, heating to 50 ℃ from 25 ℃ at a heating rate of 0.1 ℃/min, uniformly stirring, and homogenizing for 8min (wherein, the homogenization comprises a first homogenization and a second homogenization which are sequentially and continuously carried out, the homogenization pressure of the first homogenization is 50MPa, the homogenization pressure of the second homogenization is 52MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.5), so as to prepare the capsule core mixed solution.

The formula for calculating the embedding rate is as follows:

Under the condition, the embedding rate of the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin is up to 91.88 percent, which shows that the capsule wall has good embedding effect on the capsule core and can effectively prevent the activity of natural compound ingredients from losing during storage.

Example 4

1) The capsule wall material comprises 10g of calcium alginate, 5g of agar, 5g of CI 778911 g of CI 770191 g of CI 774911.5 g of CI, 2.5g of phenoxyethanol, 5g of p-hydroxyacetophenone and 174g of caprylic/capric triglyceride. The capsule wall material is added into 800mL deionized water, heated and stirred uniformly at 80 ℃ to obtain capsule wall mixed liquid.

2) The capsule core material comprises 600g of lactobacillus/rice fermentation product, 10g of schizosaccharomyces cerevisiae fermentation product lysate, 15g of acetyl hexapeptide-8, 15g of palmitoyl tripeptide-1, 15g of palmitoyl tetrapeptide-7, 10g of donkey-hide gelatin, 15g of polysorbate-20, 15g of xanthan gum, 15g of 1, 2-hexanediol, 15g of p-hydroxyacetophenone, 120g of glycerol, 120g of butanediol and 35mL of water. Mixing the capsule core materials, heating to 50 ℃ from 25 ℃ at a heating rate of 0.1 ℃/min, uniformly stirring, and homogenizing for 8min (wherein, the homogenization comprises a first homogenization and a second homogenization which are sequentially and continuously carried out, the homogenization pressure of the first homogenization is 50MPa, the homogenization pressure of the second homogenization is 52MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.5), so as to prepare the capsule core mixed solution.

The formula for calculating the embedding rate is as follows:

Under the condition, the embedding rate of the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin is up to 91.36 percent, which shows that the capsule wall has good embedding effect on the capsule core and can effectively prevent the activity of natural compound ingredients from losing during storage.

Example 5

1) The capsule wall material comprises 10g of calcium alginate, 40g of agar, 778912 g of CI, 770192 g of CI, 774911.5 g of CI, 2.5g of phenoxyethanol, 2.5g of p-hydroxyacetophenone and 339.5g of caprylic/capric triglyceride. The capsule wall material is added into 600mL deionized water, heated and stirred uniformly at 80 ℃ to obtain capsule wall mixed liquid.

2) The capsule core material comprises 665g of lactobacillus/rice fermentation product, 10g of schizosaccharomyces cerevisiae fermentation product lysate, 15g of acetyl hexapeptide-8, 15g of palmitoyl tripeptide-1, 15g of palmitoyl tetrapeptide-7, 100g of donkey-hide gelatin, 15g of polysorbate-20, 15g of xanthan gum, 15g of 1, 2-hexanediol, 15g of p-hydroxyacetophenone, 10g of glycerol, 10g of butanediol and 100mL of water. Mixing the capsule core materials, heating to 50 ℃ from 25 ℃ at a heating rate of 0.1 ℃/min, uniformly stirring, and homogenizing for 8min (wherein, the homogenization comprises a first homogenization and a second homogenization which are sequentially and continuously carried out, the homogenization pressure of the first homogenization is 50MPa, the homogenization pressure of the second homogenization is 52MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.5), so as to prepare the capsule core mixed solution.

The formula for calculating the embedding rate is as follows:

Under the condition, the embedding rate of the repairing and moistening hydrogel microcapsule containing the donkey-hide gelatin is up to 93.26 percent, which shows that the capsule wall has good embedding effect on the capsule core and can effectively prevent the activity of natural compound ingredients from losing during storage.

Example 6

The procedure of example 1 was followed, except that CI77891, CI 770192, and CI77491 were not used, and the resulting repairing and moisturizing hydrogel microcapsules were spherical, the wall of the capsule was translucent, and the core was translucent.

Example 7

The procedure is as in example 1, except that the homogenization is carried out in one step under the following conditions: homogenizing under 55MPa for 3 min.

Example 8

The procedure is as in example 1, except that, in the heat treatment in step 2): the heating rate was 0.5 ℃/min.

Example 9

The procedure is as in example 1, except that, in the heat treatment in step 2): the heating rate was 0.05 ℃/min.

Comparative example 1

The procedure is as in example 1, except that 10g of calcium alginate, 20g of agar, are exchanged for 30g of calcium alginate.

Comparative example 2

The procedure is as in example 1, except that 10g of calcium alginate and 20g of agar are replaced by 30g of agar.

Comparative example 3

The procedure is as in example 1, except that 10g of calcium alginate and 20g of agar are exchanged for 30g of gum arabic.

Comparative example 4

The procedure is as in example 1, except that in step 2) the materials are mixed at 25 ℃ and heated to 40 ℃.

Comparative example 5

The procedure is as in example 1, except that in step 2) the materials are mixed at 25 ℃ and heated to 75 ℃.

Comparative example 6

The procedure is as in example 1, except that in step 2), homogenization is carried out in one step under the following conditions: homogenizing under 60MPa for 2 min.

Comparative example 7

The procedure is as in example 1, except that in step 2), homogenization is carried out in one step under the following conditions: homogenizing under homogenizing pressure of 40MPa for 15 min.

Detection example 1

To better illustrate the applicability of the present invention, the donkey-hide gelatin anti-aging hydrogel microcapsules prepared in the above examples and comparative examples of the present invention were added to the anti-aging eye cream in an amount of 3 wt%, and stability and safety tests were performed on the anti-aging eye cream to which the donkey-hide gelatin anti-aging hydrogel microcapsules were added.

The preparation process of the anti-aging eye cream comprises the following steps:

adding 50g of glycerin, 100g of butanediol, 10g of panthenol, 30g of glycerin polyacrylate/glycerin (a commercial product of Guangzhou Huilan Biotech Co., Ltd. with the trade name of luba oil), 0.5g of disodium EDTA and 0.5g of sodium hyaluronate into 377g of water, heating to 80 ℃, and uniformly mixing to obtain a first mixture;

100g of C12-20 acid PEG-8 ester (commercially available from Guangzhou Fuyu vitamin science Co., Ltd.), 50g of caprylic/capric triglyceride, 70g of cocoyl-caprylic/capric acid ester (commercially available from Guangzhou Ruizhou chemical science Co., Ltd.), 50g of squalane, 30g of cetyl palmitate (commercially available from Guangzhou Ruizhou chemical science Co., Ltd.), 30g of bis-diglycerol polyacyladipate-2 (commercially available from Guangzhou Cheng trade Co., Ltd.), 10g of tocopherol acetate/ceramide 3/hydrogenated lecithin/cholesterol (commercially available from Shanghai Honghui Cheng GmbH Co., Ltd., trade name PresomeR-3), 10g of phytosterol oleate were mixed by stirring at 80 ℃ to obtain a second mixture, and the second mixture was added to the first mixture and emulsified by stirring for 15min, homogenizing until the material body is uniform to obtain a third mixture;

30g of polydimethylsiloxane/vinyldimethylsiloxane crosspolymer/cyclopenta-polydimethylsiloxane (commercially available under the trade name of silicon elastomer from Wanlu chemical Co., Ltd., Guangzhou) was added to the third mixture, stirred until homogeneous, and homogenized until homogeneous to obtain a fourth mixture.

When the temperature of the fourth mixture is reduced to 60 ℃, 5g of 1, 2-hexanediol, 4g of p-hydroxyacetophenone, and 4g of butanediol/1, 2-hexanediol/octanohydroxamic acid (commercially available from Shanghai Dry chemical Co., Ltd. under the name BHC) are uniformly mixed and dissolved, and then the mixture is added into the fourth mixture and uniformly mixed to obtain a fifth mixture.

When the temperature of the substrate mixture is reduced to 45 ℃,7g of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer/polyisobutene/PEG-7 Trihydroxymethyl propyl CocoPer (commercially available from SEPPIC company under the name SEPIPLUS)^TMCommercially available product of S) was stirred and mixed to obtain a sixth mixture.

Adding 10g tranexamic acid, 10g acetyl hexapeptide-8, 10g water/1, 3-propanediol/schizophyllan (a commercial product of Guangzhou Fulvin trading Co., Ltd.), 1g adenosine/water, 0.5g carnosine, 0.5g glycogen and 30g prepared donkey-hide gelatin hydrogel microcapsule into the fifth mixture, uniformly mixing, and cooling to the discharging temperature to obtain the finished product.

The storage stability is generally evaluated in accordance with GB/T29665-2013. Preservative efficacy test using international standard ISO 11930: 2012 (cosmetics-microbiology-assessment of antimicrobial protection of cosmetic products) annex B standard methods a in table b.1; the safety test adopts corresponding technical means according to the requirements of technical Specification for cosmetic safety (2015 edition) to detect the safety of heavy metals (lead, mercury, arsenic and cadmium), risk substances (diethylene glycol and dioxane) and microorganisms in the cosmetic water.

The general storage stability test results of the anti-aging eye cream added with the donkey-hide gelatin anti-aging hydrogel microcapsule prepared in example 1 are shown in table 1, and the eye cream has no obvious changes in appearance, smell and pH value in freeze-thaw cycles and heat/cold resistance tests and has storage stability.

TABLE 1

As can be seen from Table 1 above, the eye creams containing the gelatin-containing anti-aging hydrogel microcapsules prepared in examples 1 to 9 all had excellent general storage stability, whereas the eye creams containing the gelatin-containing anti-aging hydrogel microcapsules prepared in comparative examples 1 to 7 all had poor general storage stability and were difficult to use as eye cream materials.

The results of the test for the antiseptic efficacy of the anti-aging eye cream added with the donkey-hide gelatin anti-aging hydrogel microcapsule prepared in example 1 are shown in table 2.

TABLE 2

The results of the test for the preservative efficacy of the eye cream containing the microcapsule of the donkey-hide gelatin anti-aging hydrogel prepared in examples 2 to 9 and comparative examples 1 to 7 were substantially identical to those of table 2, which were measured according to the same method.

The results of detecting heavy metals and risk substances of the anti-aging eye cream added with the donkey-hide gelatin anti-aging hydrogel microcapsule prepared in example 1 are shown in table 3. In Table 3, lead, mercury, arsenic, cadmium, diethylene glycol and dioxane all meet safety standards.

TABLE 3

The heavy metal and risk substance detection results of the eye cream containing the donkey-hide gelatin anti-aging hydrogel microcapsules prepared in examples 2 to 9 and comparative examples 1 to 7 are substantially the same as those in table 3.

The results of the microbiological examination of the anti-aging eye cream added with the donkey-hide gelatin anti-aging hydrogel microcapsule prepared in example 1 are shown in table 4. The microbiological indicators in table 4 meet safety standards.

TABLE 4

The results of microbiological examination of the eye creams containing the donkey-hide gelatin anti-aging hydrogel microcapsules prepared in examples 2 to 9 and comparative examples 1 to 7 were substantially the same as those in table 4.

Detection of anti-aging effects

30 volunteers (women 25 to 50 years old without a history of skin disease and cosmetic allergy) were recruited to evaluate the effect of the eye cream. After cleaning the face of a volunteer in the morning and evening, the anti-aging eye cream prepared above is applied to eyes, and the trial time is 7 days. In the period, all volunteers do not change the original facial cleaning and skin care products and modes except the eye cream, only basic moisturizing cosmetics can be used, and cosmetics or medicines with anti-wrinkle effect are not used. Before and 7 days after the anti-aging eye cream was used, the "skin moisturization", "skin elasticity", "skin glossiness", "skin smoothness" and "general fine line condition" parameters of the eyes of the subject were evaluated by a dermatologist, and the results are shown in tables 5 and 6. The smaller the expert evaluation parameters are, the better the skin is.

The anti-aging eye cream used by the volunteers in table 5 was prepared from the donkey-hide gelatin anti-aging microcapsules prepared in example 1 according to the preparation method of the anti-aging eye cream.

TABLE 5

In Table 5, no data are shown in the numbers 22, 28-29, indicating that the volunteers were out of group for personal reasons and the data were not counted. In statistical significance, denotes P < 0.05 compared to the initial value. As can be seen from table 5, all parameters including "skin moisturization", "skin elasticity", "skin glossiness", "skin smoothness", "skin whiteness", "overall fine line condition" and "canthus wrinkles" were significantly improved after 7 days of the test eye cream use compared to the initial values.

In the same manner, 30 volunteers were recruited and examined eye creams containing the hydrogel microcapsules of donkey-hide gelatin prepared in examples 2 to 9, and the examination results of eye creams containing the hydrogel microcapsules of donkey-hide gelatin prepared in examples 2 to 3 and 6 to 9 were approximately equivalent to those in table 6, and the examination results of eye creams containing the hydrogel microcapsules of donkey-hide gelatin prepared in examples 4 to 5 were slightly inferior to those in tables of examples 1 to 2.

The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.

It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.

Claims

1. The repairing and moistening hydrogel microcapsule containing donkey-hide gelatin is characterized by comprising the following components in parts by weight: the repairing and moistening hydrogel microcapsule comprises a capsule core and a capsule wall, wherein the capsule wall is coated outside the capsule core, the average particle size of the repairing and moistening hydrogel microcapsule is 0.5-4mm, and the diameter ratio of the capsule core to the capsule wall is 1: 1-3;

2. The repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin according to claim 1, wherein the weight ratio of the calcium alginate to the agar to the phenoxyethanol to the p-hydroxyacetophenone to the caprylic/capric triglyceride to the water is 1: 1.0-2.0: 1.0-1.2: 1.0-2.0: 20-30: 65-75 parts of;

the weight ratio of the schizosaccharomyces cerevisiae fermentation product lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butanediol, water, lactobacillus/rice fermentation product lysate is 1: 0.1-1.0: 0.1-1.0: 0.1-1.0: 0.1-1.0: 2-8: 0.08-1.0: 0.08-1.0: 0.08-1.0: 2-8.0: 2-8.0: 2-6.0: 70-90.

3. The repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin according to claim 1 or 2, wherein the repairing and moisturizing hydrogel microcapsule has an average particle size of 1-3mm, and the ratio of the diameter of the capsule core to the capsule wall is 1: 1.5-2.5.

4. The repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin as claimed in claim 1 or 2, wherein the capsule wall further contains a coloring agent, and the coloring agent contains CI 77019, CI77891 and CI 77491; the weight ratio of the calcium alginate to the CI 77019 to the CI77891 to the CI77491 is 1: 0.1-0.3: 0.1-0.3: 0.05-0.15.

5. The preparation method of the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin as claimed in claim 1, wherein the preparation method comprises the following steps:

6. The method of claim 5, wherein the weight ratio of calcium alginate, agar, phenoxyethanol, p-hydroxyacetophenone, caprylic/capric triglyceride, and water is 1: 1.0-2.0: 1.0-1.2: 1.0-2.0: 20-30: 65-75 parts of;

the weight ratio of the split yeast fermentation product lysate, acetyl hexapeptide-8, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, 1, 2-hexanediol, donkey-hide gelatin, polysorbate-20, p-hydroxyacetophenone, xanthan gum, glycerol, butanediol, water and lactobacillus/rice fermentation product lysate is 1: 0.1-1.0: 0.1-1.0: 0.1-1.0: 0.1-1.0: 2-8: 0.08-1.0: 0.08-1.0: 0.08-1.0: 2-8.0: 2-8.0: 2-6.0: 70-90.

7. The preparation method according to claim 5, wherein in step 1), the average particle size of the repairing hydrogel microcapsule is 1-3mm, and the ratio of the diameter of the capsule core to the capsule wall is 1: 1.5-2.5;

preferably, in the step 2), after the mixing is finished, the system is heated to 45-65 ℃ from 15-25 ℃ at a heating rate of 0.1-0.3 ℃/min;

preferably, in step 2), the homogenization treatment is performed in a stepwise manner, and includes a first homogenization and a second homogenization which are sequentially performed in series, wherein the first homogenization pressure is 45-50MPa, the second homogenization pressure is 51-55MPa, and the time ratio of the first homogenization to the second homogenization is 1: 0.2-0.5.

8. The production method according to any one of claims 5 to 7, wherein, in step 1), CI 77019, CI77891, CI77491, calcium alginate, agar, phenoxyethanol, p-hydroxyacetophenone, caprylic/capric triglyceride, and water are mixed to obtain a capsule wall mixture; the weight ratio of the calcium alginate to the CI 77019 to the CI77891 to the CI77491 is 1: 0.1-0.3: 0.1-0.3: 0.05-0.15.

9. Use of the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin according to any one of claims 1 to 4 in preparation of an anti-aging cosmetic.

10. The use of claim 9, wherein the repairing and moisturizing hydrogel microcapsule containing donkey-hide gelatin is added in an amount of 0.1 to 8 wt% in the anti-aging cosmetic;

the anti-aging cosmetic is an anti-aging eye cream cosmetic or a face cream cosmetic.