Cell bionic micro-capsule soft bead and preparation method thereof
By biomimetic cell membrane biomimetic microcapsule soft beads, the problems of thick wall material, uncontrollable particle size, low transparency and poor stability in existing microcapsule technology are solved, and the sustained release of active ingredients is achieved It is suitable for packaging fat-soluble and water-soluble ingredients in cosmetics, improving the safety and environmental performance of the product.
Patent Information
- Application Number
- CN202411815615.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-11
- Publication Date
- 2025-01-07
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In the cosmetics field, existing microcapsule technology has problems such as thick wall material, uncontrollable particle size, low transparency, easy to lose, poor stability, high cost, insufficient recoagulation and low safety, especially fat-soluble ingredients in the skin. The application effect on the product is poor, and the product stability and aesthetics are insufficient.
Bio-source encapsulated materials are used to biomimicry the cell membrane, and cell bionic microcapsulated soft beads are prepared through pressure equilibrium, electrolyte equilibrium, concentration equilibrium and osmotic pressure equilibrium, using high-quality collagen and polysaccharide as the main soft bead membrane materials, and cured in combination with special processes. , achieve slow release and direct release, including aliphatic and water-soluble ingredients, improving stability and safety.
It realizes the sustained release effect of active ingredients, improves bioavailability and stability, extends the shelf life, enhances the stability and aesthetics of cosmetic ingredients, reduces side effects and irritation, expands the scope of application, and improves safety and environmentally friendly performance.
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Figure CN119257956A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of biomass cosmetics, and in particular to a cell bionic microcapsule bead and a preparation method thereof. Background Art
[0002] Microcapsules can be used to encapsulate various active ingredients, such as drugs, cosmetic ingredients, etc. Microcapsule technology can improve the stability, permeability and bioavailability of active ingredients, and reduce side effects and irritation. There are two main existing microcapsule preparation technologies. One is to use polymer materials such as cellulose as wall materials to encapsulate active ingredients inside. The other is to use lipid materials such as lecithin as wall materials to encapsulate active ingredients inside. Among them, using cellulose as a coating body has a thick wall material, is not easy to absorb, and has an uncontrollable particle size, which limits its application on the skin. Using lecithin as a coating body has low transparency and is easy to rancid, affecting the stability and aesthetics as a cosmetic ingredient.
[0003] Fat-soluble functional ingredients have good biological activity. Due to the influence of physicochemical properties, physiological barriers and biochemical barriers, they have poor compatibility with water, poor stability, poor permeability, short biological half-life, certain irritation, easy metabolism and fast elimination. If used in skin care products, in order to make the fat-soluble ingredients and water phases mix, it is necessary to add surfactants for emulsification so that the oil and water phases are mixed into one. If such a system is left for a long time or the storage conditions are improper, the oil and water phases will separate, which means that the product is unstable and easy to fail. Therefore, the current stock solution has a short shelf life and the effect after use is relatively poor. The poor skin feel of fat-soluble products, as well as the problems of unstable lipid encapsulation carriers on the market, high cost, insufficient recondensation, complex encapsulation carrier components and low safety, have limited the development and application of microencapsulation technology in the fields of cosmetics and medicine. Summary of the invention
[0004] In view of the above problems, one object of the present invention is to provide a method for preparing cell bionic microcapsule beads. The cell membrane is bionicized by using biological source encapsulation materials, and the active ingredients are encapsulated therein. Due to the use of pressure balance, electrolyte balance, concentration balance, osmotic pressure balance, etc., slow release can be achieved, and direct release can be achieved when kneading. The problem that traditional microcapsules cannot directly release active ingredients when kneading is solved. It also solves the problem that the wall material of traditional cellulose coatings is thick, not easy to absorb, and the particle size is uncontrollable. The problem of low transparency and easy rancidity of lecithin coatings is solved.
[0005] The second object of the present invention is to provide a cell bionic microcapsule soft bead. High-quality collagen, polysaccharide, etc. are used as the main soft bead membrane material, and a special process is used for solidification, which ensures stability while ensuring safety, and can encapsulate a variety of functional ingredients. Not only fat-soluble functional ingredients can be encapsulated, but also water-soluble functional ingredients can be encapsulated, ensuring the stability and aesthetics of using it as a cosmetic ingredient.
[0006] The first technical solution adopted by the present invention is: a method for preparing cell bionic microcapsule soft beads, characterized by comprising: Step 1: preparing the first phase and the second phase; The preparation process of the first phase includes: dissolving the film former and the preservative in deionized water, heating and stirring until there are no particles, then adding the active ingredient thereto, mixing evenly, to obtain the first phase; The preparation process of the second phase includes: dispersing the anionic gel in deionized water, ultrasonically and heating and stirring until no obvious particles are present, thereby obtaining the second phase; Step 2: Keeping the first phase in a stirring state, spraying the second phase into the first phase to form a mixed solution; Step 3: Use an acidic pH regulator to adjust the mixed solution to a first pH value, add biological enzymes thereto, stir and dissolve, and then use an alkaline pH regulator to adjust the pH value to a second pH value, perform carbohydrate enzyme bridging to form a stable shell, and grade and screen to obtain cell bionic microcapsule beads.
[0007] Preferably, the preservative includes one or more of phenoxyethanol, 1,2-pentanediol, 1,2-hexanediol, butylene glycol, caprylyl glycol, ethylhexylglycerin, p-hydroxyacetophenone, and caprylhydroxamic acid; The film-forming agent comprises one or more of chitosan gel, gelatin, cation-modified gel Tremella polysaccharide, tamarind gum, psyllium gum, and hyaluronic acid.
[0008] Furthermore, the cation-modified gel Tremella polysaccharide is prepared by dissolving 10 wt % of Tremella polysaccharide and 1 wt % of zinc gluconate in 89 wt % of deionized water, followed by ultrasonic treatment and drying.
[0009] Preferably, the active ingredient includes one or more of lithospermum oil, ethylhexyl palmitate, tocopherol, ascorbyl tetraisopalmitate, ceramide EOP, ceramide NS / ceramide NG, ceramide NP, ceramide AS, ceramide AP, phytol, hydrogenated polyisobutene, lycopene, guaiazulene, ethylhexyl methoxycinnamate, octocrylene, diethylaminobenzoyl hexyl benzoate, butyl methoxydibenzoylmethane hexyl ester, ethylhexyl triazone and bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0010] Preferably, the anionic gel comprises one or more of gum arabic, sodium alginate, carrageenan and xanthan gum.
[0011] Preferably, the biological enzyme includes one or more of TG transglutaminase, tyrosinase, papain, laccase, peroxidase, sulfhydryl oxidase, lipoxygenase and glutamyl endopeptidase.
[0012] Preferably, the acidic pH regulator includes one or more of citric acid, lactic acid, salicylic acid, tartaric acid, and malic acid; The alkaline pH regulator includes one or more of sodium hydroxide, potassium hydroxide, tromethamine, arginine, aminomethyl propanol, and triethanolamine.
[0013] Preferably, the bridging time of the carbohydrase is 48 hours.
[0014] Preferably, the first pH value is 4.5, and the second pH value is 5.5.
[0015] The second technical solution adopted by the present invention is: a cell bionic microcapsule soft bead.
[0016] Beneficial effects of the above technical solution: (I) The cell bionic microcapsule beads provided by the present invention have a good sustained release effect, which can prolong the residence time of active ingredients on the skin and improve their bioavailability. The cell membrane is bionicized with biological source encapsulation materials, and the active ingredients are encapsulated therein. Due to the use of pressure balance, electrolyte balance, concentration balance, osmotic pressure balance, etc., slow release can be achieved, and direct release can be achieved when rubbing. This encapsulation method not only improves the stability, permeability and bioavailability of active ingredients, but also reduces side effects and irritation, and improves user experience.
[0017] (II) The cell bionic microcapsule beads provided by the present invention have good stability, are not easy to become rancid, oxidized and degraded, extend the shelf life and improve the commercial value. At the same time, due to the use of bio-source encapsulation materials, the microcapsules in this technical solution have good biodegradability, will not pollute the environment, and have good environmental performance.
[0018] (III) The biogenic reticular polysaccharide spheroidization technology adopted in the present invention can encapsulate active ingredients, solving the defects of traditional categories. This technology can not only control the particle size and improve the absorption rate, but also improve the transparency and stability, enhancing the stability and aesthetics as a cosmetic ingredient. The preparation process of the cell bionic microcapsule soft bead encapsulation carrier of this technology can not only encapsulate fat-soluble functional ingredients, but also encapsulate water-soluble functional ingredients, expanding the scope of application. At the same time, due to the use of biogenic encapsulation materials, it has good biocompatibility, will not cause irritation and allergic reactions to the skin, and improves safety. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 A microscope image of a cell bionic microcapsule soft bead provided in one embodiment of the present invention; Figure 2 This is a graph of chicken embryo test results provided by an embodiment of the present invention. DETAILED DESCRIPTION
[0020] The following is a further detailed description of the implementation methods of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than an exhaustive list of all the embodiments. It should be noted that the embodiments and features in the embodiments of the present application can be combined with each other without conflict.
[0021] The terms "first", "second", etc. (if any) in the specification and claims are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that the terms used in this way are interchangeable where appropriate so that the embodiments described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, for example, a process, method, system, product, or device that includes a series of steps or units is not necessarily limited to those steps or units that are clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products, or devices.
[0022] It should be understood that the term "and / or" used in this article is only a description of the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in this article generally indicates that the associated objects before and after are in an "or" relationship.
[0023] 1. Raw materials and auxiliary materials information Component A: preservative, film-forming agent.
[0024] The preservatives are one or more of phenoxyethanol, 1,2-pentanediol, 1,2-hexanediol, butylene glycol, caprylyl glycol, ethylhexylglycerin, p-hydroxyacetophenone, and caprylhydroxamic acid.
[0025] The film-forming agent is a cationic gel including: chitosan gel, gelatin, cationically modified gel tremella polysaccharide (the cationically modified gel tremella polysaccharide is obtained by dissolving 10wt% tremella polysaccharide and 1wt% zinc gluconate in 89wt% deionized water, ultrasonically treating for 5 minutes and then drying), tamarind gum, psyllium gum, and one or more of hyaluronic acid.
[0026] Component B (active ingredients): one or more of lithospermum oil, ethylhexyl palmitate, tocopherol (vitamin E), ascorbyl tetraisopalmitate, ceramide EOP, ceramide NS / ceramide NG, ceramide NP, ceramide AS, ceramide AP, phytol, hydrogenated polyisobutene, lycopene, guaiazulene, ethylhexyl methoxycinnamate, octocrylene, diethylaminobenzoyl hexyl benzoate, butyl methoxydibenzoylmethane hexyl ester, ethylhexyl triazone, and bis-ethylhexyloxyphenol methoxyphenyl triazine.
[0027] Component C: Anionic gel is one or more of gum arabic, sodium alginate, carrageenan and xanthan gum.
[0028] Other components: deionized water, biological enzyme, acidic pH regulator, alkaline pH regulator.
[0029] The biological enzyme is one or more of TG glutaminase, tyrosinase, papain, laccase, peroxidase, sulfhydryl oxidase, lipoxygenase and glutamyl endopeptidase.
[0030] Acidic pH adjuster: one or more of citric acid, lactic acid, salicylic acid, tartaric acid, and malic acid.
[0031] Alkaline pH adjuster: one or more of sodium hydroxide, potassium hydroxide, tromethamine, arginine, aminomethyl propanol, and triethanolamine.
[0032] The preparation method of cell bionic microcapsule soft beads comprises the following steps: Preparation of phase A (first phase) and phase C (second phase): Preparation of phase A: Dissolve the film former and preservative in deionized water, heat to 60-80°C and stir until there are no particles to obtain a film former aqueous solution. Then add component B and ultrasonicate for 5 minutes until component B is evenly dispersed in the film former aqueous solution to obtain phase A for later use. The heating temperature is specifically selected according to the different components of B.
[0033] Preparation of phase C: Disperse the anionic gel evenly in deionized water, sonicate for 5 min, heat to 50°C and stir until no obvious particles remain to obtain phase C for later use.
[0034] Mixture of phase A and phase C: Phase C is sprayed into phase A through a high-pressure air flow atomizer, and phase A is kept in a stirring state to form a mixed solution.
[0035] Shell formation: The acidic pH regulator adjusts the pH of the mixed solution to pH 4.5. The biological enzyme is added thereto, stirred and dissolved, and the pH is adjusted to 5.5 using an alkaline pH regulator. The sugar enzyme bridges for 48 hours to form a stable shell. After the enzymatic reaction is completed, the mixture is graded and sieved to obtain the cell biomimetic microcapsule beads.
[0036] Prepare component A, component B, component C and other raw materials as shown in Tables 1 to 3, and then prepare the cell bionic microcapsule soft beads of Examples 1 to 5 according to the preparation method of cell bionic microcapsule soft beads. The components used in Examples 1 to 5 are shown in Table 4. They are marked as cell bionic microcapsule soft beads 1 to cell bionic microcapsule soft beads 5, respectively.
[0037] Table 1 Raw materials and weight ratio of component A
[0038] Table 2 Raw materials and weight ratio of component B
[0039] Table 3 Raw materials and weight ratios of component C and other components
[0040] Table 4 Raw materials for preparing cell biomimetic microcapsule beads
[0041] Example 1 Preparation of phase A: Dissolve component A in deionized water, heat to 60-80°C and stir until there are no particles to obtain a film-forming agent aqueous solution. Then add component B and sonicate for 5 minutes until component B is evenly dispersed in the film-forming agent aqueous solution to obtain phase A for later use.
[0042] The anionic gel was evenly dispersed in deionized water, ultrasonicated for 5 min, heated to 50°C and stirred until no obvious particles were present to obtain phase C for later use.
[0043] Phase C is sprayed into phase A through a high-pressure air flow atomizer, and phase A is kept in a stirring state to form a mixed solution.
[0044] The acidic pH regulator adjusts the pH of the mixed solution to pH 4.5. The biological enzyme is added thereto, stirred and dissolved, and the pH is adjusted to 5.5 using an alkaline pH regulator. The sugar enzyme bridges for 48 hours to form a stable shell. After the enzymatic reaction is completed, the mixture is graded and sieved to obtain the cell biomimetic microcapsule soft beads.
[0045] Example 2 Preparation of phase A: Dissolve component A in deionized water, heat to 60-80°C and stir until there are no particles to obtain a film-forming agent aqueous solution. Then add component B and sonicate for 5 minutes until component B is evenly dispersed in the film-forming agent aqueous solution to obtain phase A for later use.
[0046] The anionic gel was evenly dispersed in deionized water, ultrasonicated for 5 min, heated to 50°C and stirred until no obvious particles were present to obtain phase C for later use.
[0047] Phase C is sprayed into phase A through a high-pressure air flow atomizer, and phase A is kept in a stirring state to form a mixed solution.
[0048] The acidic pH regulator adjusts the pH of the mixed solution to pH 4.5. The biological enzyme is added thereto, stirred and dissolved, and the pH is adjusted to 5.5 using an alkaline pH regulator. The sugar enzyme bridges for 48 hours to form a stable shell. After the enzymatic reaction is completed, the mixture is graded and sieved to obtain the cell biomimetic microcapsule soft beads II.
[0049] Example 3 Preparation of phase A: Dissolve component A in deionized water, heat to 60-80°C and stir until there are no particles to obtain a film-forming agent aqueous solution. Then add component B and sonicate for 5 minutes until component B is evenly dispersed in the film-forming agent aqueous solution to obtain phase A for later use.
[0050] The anionic gel was evenly dispersed in deionized water, ultrasonicated for 5 min, heated to 50°C and stirred until no obvious particles were present to obtain phase C for later use.
[0051] Phase C is sprayed into phase A through a high-pressure air flow atomizer, and phase A is kept in a stirring state to form a mixed solution.
[0052] The acidic pH regulator adjusts the pH of the mixed solution to pH 4.5. The biological enzyme is added thereto, stirred and dissolved, and the pH is adjusted to 5.5 using an alkaline pH regulator. The sugar enzyme bridges for 48 hours to form a stable shell. After the enzymatic reaction is completed, the mixture is graded and sieved to obtain the cell biomimetic microcapsule soft beads III.
[0053] Example 4 Preparation of phase A: Dissolve component A in deionized water, heat to 60-80°C and stir until there are no particles to obtain a film-forming agent aqueous solution. Then add component B and sonicate for 5 minutes until component B is evenly dispersed in the film-forming agent aqueous solution to obtain phase A for later use.
[0054] The anionic gel was evenly dispersed in deionized water, ultrasonicated for 5 min, heated to 50°C and stirred until no obvious particles were present to obtain phase C for later use.
[0055] Phase C is sprayed into phase A through a high-pressure air flow atomizer, and phase A is kept in a stirring state to form a mixed solution.
[0056] The acidic pH regulator adjusts the pH of the mixed solution to pH 4.5. The biological enzyme is added thereto, stirred and dissolved, and the pH is adjusted to 5.5 using an alkaline pH regulator. The sugar enzyme bridges for 48 hours to form a stable shell. After the enzymatic reaction is completed, the mixture is graded and sieved to obtain the cell biomimetic microcapsule soft beads IV.
[0057] Example 5 Preparation of phase A: Dissolve component A in deionized water, heat to 60-80°C and stir until there are no particles to obtain a film-forming agent aqueous solution. Then add component B and sonicate for 5 minutes until component B is evenly dispersed in the film-forming agent aqueous solution to obtain phase A for later use.
[0058] The anionic gel was evenly dispersed in deionized water, ultrasonicated for 5 min, heated to 50°C and stirred until no obvious particles were present to obtain phase C for later use.
[0059] Phase C is sprayed into phase A through a high-pressure air flow atomizer, and phase A is kept in a stirring state to form a mixed solution.
[0060] The acidic pH regulator adjusts the pH of the mixed solution to pH 4.5. The biological enzyme is added thereto, stirred and dissolved, and the pH is adjusted to 5.5 using an alkaline pH regulator. The sugar enzyme bridges for 48 hours to form a stable shell. After the enzymatic reaction is completed, the mixture is graded and sieved to obtain the cell biomimetic microcapsule soft beads V.
[0061] Comparative Example 1 Compare with the formulation and preparation method of lightweight essential oil with micro-gel beads.
[0062] The ingredients of the group A preparation include water, allantoin, butylene glycol, glycerin, betaine, parahydroxyacetophenone, 1,2-pentanediol, glyceryl polyacrylate composition, polybutylene glycol-8 / 5 / 3 glycerol and glyceryl polyether-26; the ingredients of the group B preparation include carbomer and sodium acrylate copolymer composition, the ingredients of the group C preparation include arginine and water, the ingredients of the group D preparation include 1,2-hexanediol and rose composition, the ingredients of the group E preparation include cyclopentasiloxane composition, and the ingredients of the group F preparation include carmine, tartrazine, lactobacillus / soy milk fermentation product filtrate composition, and creatine.
[0063] First, weigh the materials of the preparation of group A in sequence and add them into the main emulsifying pot, then add the carbomer, the sodium acrylate copolymer composition, and the cyclopentasiloxane composition into the vortex of the water flow by suction at a low speed, and then homogenize at a high speed for 10 minutes; Then disperse NG with A100 and add it into the main emulsification pot, stir and heat to 80-85℃, keep warm for 20 minutes, stir and cool down; When the temperature drops to 70-75°C, add the dissolved Group C preparation and stir to cool down; When the temperature drops to 40-45°C, add the preparations of group D and group F, stir evenly, and filter with a 400-mesh filter cloth; Add the E group preparation and stir slowly.
[0064] The components of the group A preparation are in the following percentage ratios: water (59.36%), allantoin (0.2%), butylene glycol (5.8%), glycerol (5%), betaine (5%), p-hydroxyacetophenone (0.3%), 1,2-pentanediol (0.5%), glycerol polyacrylate composition (2%), polybutylene glycol-8 / 5 / 3 The ingredients of the group B preparation are carbomer (0.12%) and sodium acrylate copolymer composition (0.08%), the ingredients of the group C preparation are arginine (0.09%) and water (1%), the ingredients of the group D preparation are 1,2-hexanediol (0.05%) and rose composition (10%), the ingredients of the group E preparation are cyclopentasiloxane composition (5%), the ingredients of the group F preparation are carmine (0.0003%), tartrazine (0.0002%), lactobacillus / soy milk fermentation product filtrate composition (0.001%), and creatine (0.001%).
[0065] Specifically, the glyceryl polyacrylate composition (2%) includes water (49%), glyceryl polyacrylate (50%), phenoxyethanol (0.8%), and ethylhexylglycerin (0.2%); the glyceryl polyether-26 composition (3%) includes water (40%), butylene glycol (30%), glyceryl polyether-26 (20%), 1,2-hexanediol (3%), β-glucan (3%), glycerol (2.49%), sodium hyaluronate (1%), caprylyl glycol (0.5%), and sodium benzoate (0.05%); the sodium acrylic acid (ester) copolymer composition (0.08%) includes sodium acrylic acid (ester) copolymer (80%) and red algae extract (20%); the rose flower composition (1 0%), including rose water (90%), propylene glycol (9.2%), caprylhydroxamic acid, glyceryl caprylate and 1,2-pentanediol (total 0.5%), and parahydroxyacetophenone (0.3%); the cyclopentasiloxane composition (5%) includes cyclopentasiloxane (40%), water (10%), squalane (40%), gelatin (4%), gum arabic (4%), solvent green (0.01%), 1,2-hexanediol (1%), and caprylyl glycol (0.98%); the lactobacillus / soy milk fermentation product filtrate composition (0.001%) includes water (78%), lactobacillus / soy milk fermentation product filtrate (10%), butylene glycol (10%), and 1,2-pentanediol (2%).
[0066] Comparative Example 2 The invention is compared with a retinol derivative oily gel bead, a skin care composition containing the oily gel bead, and a preparation method thereof.
[0067] Mix dextrin fatty acid ester and emollient oil compatible with silicone oil according to a proportion, stir evenly, and obtain a dispersion; Adding other ingredients except the retinol derivative into the dispersion, mixing and stirring evenly; Heat to 80-90℃, keep warm and stir until the material is completely dissolved; Add the retinol derivative to the mixed solution in step 3 and stir evenly; The solution obtained in step 4 is added into 2 to 5 times the weight of water at a temperature of 80 to 90° C. and stirred and cooled until spherical oil droplets are condensed.
[0068] Detection and evaluation of cell biomimetic microcapsule beads 1. Observe product properties The cell bionic microcapsule beads prepared by the present invention were observed by electron microscope. The cell bionic microcapsule beads of Example 1 were as follows: Figure 1As shown, the cell bionic microcapsule beads provided by the present invention appear as uniform and transparent tiny microbeads, and the particle size distribution includes 0.02-2.0 mm.
[0069] 2. Safety evaluation Based on: "Technical Specifications for Safety of Cosmetics" (2015 edition), with clinical medicine as the theoretical basis, a specific experimental population is formed into a test group, and a patch test is conducted on the designated parts of the subjects to determine the potential possibility of adverse reactions of cosmetics to human skin. Select qualified patch test materials. Put the test substance into the patch tester, with an amount of about 0.020 g to 0.025 g (solid or semi-solid) or 0.020 mL to 0.025 mL (liquid, which can be dripped on the filter paper attached to the patch tester and placed in the patch tester).
[0070] When the test substance is the original cosmetic final product, the control well is a blank control (no substance is placed in it). When the test substance is a diluted cosmetic, the diluent of the cosmetic is used in the control well.
[0071] Apply the patch tester containing the test substance to the back or curved forearm of the subject with non-irritating tape, and press lightly with the palm of the hand to make it evenly adhere to the skin for 24 hours.
[0072] Observe the skin reaction 30 minutes after the test patch tester is removed and the indentation disappears. If the result is negative, observe again 24 hours and 48 hours after the patch test. Record the reaction results according to Table 5 (Grading Standards for Adverse Skin Reactions).
[0073] Table 5 Grading table for adverse skin reactions
[0074] Interpretation of skin occlusive patch test results: If more than 5 out of 30 subjects experience Grade 1 adverse skin reactions, or more than 2 subjects experience Grade 2 adverse skin reactions, or any Grade 3 or above adverse skin reaction occurs, the test substance is judged to have an adverse reaction to the human body.
[0075] Table 6 Safety evaluation results of cell bionic microcapsule beads
[0076] 3. Stability test Cold resistance: Place the sealed sample in a -10±1℃ environment for two weeks. After returning to room temperature, compare the appearance with the sample stored at room temperature (25±3℃).
[0077] Lighting: Place the sealed sample under light with an intensity of 1.5×106 Lux .hr for two weeks. After returning to room temperature, compare the appearance with the sample stored at room temperature (25±3℃).
[0078] Heat resistance: Place the sealed sample in a 48±1℃ environment for two weeks. After returning to room temperature, compare the appearance with the sample stored at room temperature (25±3℃).
[0079] The test results are shown in Table 7.
[0080] Table 7 Stability test results of cell bionic microcapsule beads
[0081] Note: √Stable 4. Sensory evaluation The essences prepared in Examples 1-5 and Comparative Examples 1-2 were subjected to a sensory evaluation test. Ten trained sensory assessors were selected to conduct separate evaluations in a separate room. Each indicator was scored from 0 to 10 points according to the sensory intensity from low to high. 20 μL of the sample was taken each time and applied in circles on the inner side of the forearm. After applying 20 circles, the lightness, slipperiness, and freshness of the sample were evaluated. After waiting for 2 minutes, the absorption speed, skin moisturization, and the residual amount of the sample on the skin were evaluated. The test results are shown in Table 8.
[0082] Table 8 Sensory evaluation results of cell bionic microcapsule beads
[0083] 5. Based on the above embodiments and comparative examples, this embodiment provides a test method for testing the transdermal absorption rate of the composition obtained in the above embodiments and comparative examples to evaluate the application effect of the composition in cosmetics.
[0084] Test material: pig skin for experiment.
[0085] Test reagents: ultrapure water, methanol, sodium chloride, acetonitrile, etc.
[0086] Experimental instruments: Franz diffuser, high performance liquid chromatograph.
[0087] Test method: Transdermal test using Franz diffusion method The steps include: 1) Take out the purchased and stored pig skin and cut it into appropriate sizes for later use; 2) One of the pig skins was washed and left untreated as a blank control group; 3) After washing the other prepared pig skin, fix it between the supply tank and the diffusion tank, and place the skin with the stratum corneum layer facing upwards, place the composition prepared in the above embodiments and comparative examples on the surface of the stratum corneum, and the bottom surface of the skin is in contact with the liquid in the diffusion tank, adjust the temperature and stirring speed of the water bath system, and exhaust all bubbles; 4) maintaining the composition in contact with the stratum corneum of pig skin for a certain period of time, and collecting the receiving solution at different time points; and selecting a high performance liquid chromatography method to detect the receiving solution according to the characteristics of the target component; 5) Set the experimental parameters of HPLC and perform detection and analysis on the receiving fluid. Each group should be repeated at least three times to improve the accuracy of the detection and analysis results. 6) By detecting the changes in the target component content in the receiving fluid collected at different time points, the transdermal absorption status of the target component can be reflected; 7) In this experiment, pig skin was selected. After a 24-h in vitro transdermal experiment, the analysis results were obtained by high performance liquid chromatography (HPLC).
[0088] Table 9 Transdermal absorption test results of cell bionic microcapsule beads
[0089] It can be seen from Table 9 above that the permeability of the composition obtained in Examples 1-5 is between 75% and 91%, and the permeability of the composition obtained in Comparative Examples 1-3 is between 58% and 69%; the permeability of the composition obtained in Examples 1-4 is between 81% and 93%, and the permeability of the composition obtained in Comparative Examples 1-2 is between 60% and 71%; Therefore, the composition obtained by the preparation method provided by the present invention has a better permeability effect.
[0090] In summary, the present invention can encapsulate ceramide and promote permeability by using the cell bionic microcapsule microbeads required by the patent; the large and medium molecules in the encapsulation carrier can form a membrane on the epidermis of the skin, generate pressure, and allow small molecules to penetrate into the deep layer, further promoting permeability; the bionic microcapsule provided by the present invention has an excellent prospect in the application of cosmetics. Therefore, the present invention effectively overcomes various shortcomings in the prior art and has a high industrial utilization value.
[0091] 6. Evaluation of content protection The protective effect of the contents of the cell bionic microcapsule beads was evaluated, and the results of the protective effect evaluation are shown in Table 10.
[0092] In the comparative test, the unencapsulated sample (indicated by 0 in the Encapsulated or Not column) is compared with the encapsulated sample (indicated by 1 in the Encapsulated or Not column).
[0093] Test conditions: 40℃±2℃, 75%RH (BPS-250CL constant temperature and humidity chamber), 25℃±2℃, 60%RH (BSC-250CL constant temperature and humidity chamber), frozen (-15~-20℃ refrigerator).
[0094] Table 10 Evaluation results of the protective properties of the contents of cell bionic microcapsules
[0095] Chicken embryo test The test was carried out in accordance with the relevant requirements of "SN / T 2329-2009 Chicken chorioallantoic membrane test for eye irritation / corrosion of cosmetics". The results are as follows Figure 2 As shown, the cell bionic microcapsule beads prepared by Examples 1 and 3 of the present invention were selected for implementation, and the toxicity of the chicken embryo chorioallantoic membrane was not changed. The chicken embryo chorioallantoic membrane produced and developed normally. It can be seen that the cell bionic microcapsule beads provided by the present invention are safe and non-irritating to use in skin care products.
[0096] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not limitations on the implementation methods of the present invention. For ordinary technicians in the relevant field, other different forms of changes or modifications can be made on the basis of the above description. It is impossible to list all the implementation methods here. All obvious changes or modifications derived from the technical solution of the present invention are still within the protection scope of the present invention.
Claims
1. A method for preparing cell bionic microcapsule beads, characterized in that: include: Step 1: preparing the first phase and the second phase; The preparation process of the first phase includes: dissolving the film former and the preservative in deionized water, heating and stirring until there are no particles, then adding the active ingredient thereto, mixing evenly, to obtain the first phase; The preparation process of the second phase includes: dispersing the anionic gel in deionized water, ultrasonically and heating and stirring until no obvious particles are present, thereby obtaining the second phase; Step 2: Keeping the first phase in a stirring state, spraying the second phase into the first phase to form a mixed solution; Step 3: Use an acidic pH regulator to adjust the mixed solution to a first pH value, add biological enzymes thereto, stir and dissolve, and then use an alkaline pH regulator to adjust the pH value to a second pH value, perform carbohydrate enzyme bridging to form a stable shell, and grade and screen to obtain cell bionic microcapsule beads.
2. The method for preparing the cell bionic microcapsule beads according to claim 1, characterized in that: The preservative includes one or more of phenoxyethanol, 1,2-pentanediol, 1,2-hexanediol, butylene glycol, caprylyl glycol, ethylhexylglycerin, p-hydroxyacetophenone, and caprylhydroxamic acid; The film-forming agent comprises one or more of chitosan gel, gelatin, cation-modified gel Tremella polysaccharide, tamarind gum, psyllium gum, and hyaluronic acid.
3. The method for preparing the cell bionic microcapsule beads according to claim 2, characterized in that: The cation-modified gel Tremella polysaccharide is prepared by dissolving 10 wt% of Tremella polysaccharide and 1 wt% of zinc gluconate in 89 wt% of deionized water, and then drying after ultrasonication.
4. The method for preparing cell bionic microcapsule beads according to claim 1, characterized in that: The active ingredients include one or more of lithospermum oil, ethylhexyl palmitate, tocopherol, ascorbyl tetraisopalmitate, ceramide EOP, ceramide NS / ceramide NG, ceramide NP, ceramide AS, ceramide AP, phytol, hydrogenated polyisobutene, lycopene, guaiazulene, ethylhexyl methoxycinnamate, octocrylene, diethylaminobenzoyl hexyl benzoate, butyl methoxydibenzoylmethane hexyl ester, ethylhexyl triazone and bis-ethylhexyloxyphenol methoxyphenyl triazine.
5. The method for preparing cell bionic microcapsule beads according to claim 1, characterized in that: The anionic gel includes one or more of gum arabic, sodium alginate, carrageenan and xanthan gum.
6. The method for preparing cell bionic microcapsule beads according to claim 1, characterized in that: The biological enzymes include one or more of TG glutaminase, tyrosinase, papain, laccase, peroxidase, sulfhydryl oxidase, lipoxygenase and glutamyl endopeptidase.
7. The method for preparing cell bionic microcapsule beads according to claim 1, characterized in that: The acidic pH regulator includes one or more of citric acid, lactic acid, salicylic acid, tartaric acid, and malic acid; The alkaline pH regulator includes one or more of sodium hydroxide, potassium hydroxide, tromethamine, arginine, aminomethyl propanol, and triethanolamine.
8. The method for preparing cell bionic microcapsule beads according to claim 1, characterized in that: The bridging time of the glycosidase is 48h.
9. The method for preparing cell bionic microcapsule beads according to claim 1, characterized in that: The first pH value is 4.5, and the second pH value is 5.
5.
10. A cell bionic microcapsule bead prepared by the method according to any one of claims 1 to 9.
Citation Information
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