CN114652636A - Anti-wrinkle repair composition, preparation method thereof and cosmetic containing composition - Google Patents
Anti-wrinkle repair composition, preparation method thereof and cosmetic containing composition Download PDFInfo
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- CN114652636A CN114652636A CN202210233396.9A CN202210233396A CN114652636A CN 114652636 A CN114652636 A CN 114652636A CN 202210233396 A CN202210233396 A CN 202210233396A CN 114652636 A CN114652636 A CN 114652636A
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- linoleic acid
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Classifications
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/361—Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides thereof
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- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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Abstract
The invention discloses an anti-wrinkle repairing composition, a preparation method thereof and a cosmetic containing the composition, wherein the preparation method of the anti-wrinkle repairing composition comprises the steps of firstly preparing colloid granular linoleic acid modified chitosan, then dissolving the obtained linoleic acid modified chitosan in water, and then adding a water-soluble skin conditioner to obtain a water phase; and then dissolving the vitamin A and/or the vitamin A derivative in oil to form an oil phase, mixing and emulsifying the water phase and the oil phase to obtain a Pickering emulsion, and loading the vitamin A and/or the vitamin A derivative on the linoleic acid modified chitosan to protect the vitamin A and/or the vitamin A derivative from being affected by the external environment to lose efficacy, and further control the release of the vitamin A and/or the vitamin A derivative to better exert the efficacy. The composition can be used as one of raw materials of cosmetics, and the Pickering emulsion has better compatibility and stability, and can be used for constructing multifunctional cosmetics.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to an anti-wrinkle repair composition, a preparation method thereof and a cosmetic containing the composition.
Background
Vitamin A is a fat-soluble vitamin, also called as retinol, which is essential for keeping the skin epithelial tissue healthy, but the structure of vitamin A contains more unsaturated bonds, so that vitamin A is very sensitive to visible light, ultraviolet light, oxygen and the like. The application of retinol in the formula of cosmetics has limitations (such as retinol is easy to oxidize in air, easy to inactivate under ultraviolet irradiation, insoluble in water and the like), the irritation and instability of retinol limit the addition amount of retinol in cosmetics, and simultaneously, the excellent anti-aging and anti-acne effects of retinol cannot be fully exerted.
In order to improve the solubility, stability and permeability of vitamin a and to increase its bioavailability, vectorization techniques are widely used to embed nutrients. Several nanometer carrier systems, such as liposome, micelle, nanometer emulsion, nanometer particle, etc. are popular in recent years. The liposome is a spherical vesicle formed by one or more layers of phospholipid bilayers, and can embed water-soluble active substances in an internal water phase, and embed fat-soluble substances in the bilayers, so that phospholipid molecules are easily subjected to oxidative degradation under the influence of light, high temperature, oxygen and pH. Micelles or microemulsions are colloidal particles having a hydrophobic core and a hydrophilic surface, formed spontaneously by a surfactant in an aqueous phase above the Critical Micelle Concentration (CMC), and have high specific surface area and low interfacial tension due to their extremely small size, and exhibit high stability. However, a large amount of small molecule surfactants are used in the preparation of the microemulsion, and a high concentration of the surfactant causes hemolytic toxicity, so that the application of the microemulsion is always potential safety hazard.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a preparation method of an anti-wrinkle repair composition, wherein linoleic acid modified chitosan is used as a solid emulsifier to wrap vitamin A and/or vitamin A derivatives to obtain Pickering emulsion, so that the addition of a surfactant is reduced, and the effect of protecting and slowly releasing the vitamin A and/or the vitamin A derivatives can be achieved; the second purpose of the invention is to provide an anti-wrinkle repair composition, which can reduce the irritation of vitamin A and/or vitamin A derivatives, and improve the stability and safety of the vitamin A and/or vitamin A derivatives; the invention also aims to provide a cosmetic which is prepared by taking the anti-wrinkle repairing composition as one of raw materials and has wide applicability.
One of the purposes of the invention is realized by adopting the following technical scheme:
a preparation method of the anti-wrinkle repair composition comprises the following steps:
1) mixing linoleic acid and chitosan for coupling to obtain solid granular linoleic acid modified chitosan;
2) diluting the linoleic acid modified chitosan with water to obtain a linoleic acid modified chitosan solution, and then adding a water-soluble skin conditioner and water to obtain a water phase;
3) dissolving vitamin A and/or vitamin A derivatives in oil to obtain oil phase;
4) mixing and emulsifying the water phase and the oil phase to obtain linoleic acid modified chitosan embedded vitamin A and/or vitamin A derivative Pickering emulsion, namely the anti-wrinkle repair composition.
Further, in the step 1), dissolving the chitosan in an acetic acid aqueous solution to obtain a chitosan solution, adding linoleic acid, stirring at 20-25 ℃, adding a methanol solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, reacting, adding a reaction mixture into a mixed solution of methanol and ammonia water, stirring, filtering, taking a precipitate, washing, and drying to obtain the solid linoleic acid modified chitosan.
Still further, in the step 1), the mass ratio of the chitosan to the linoleic acid is 1: (0.8 to 1); the molar ratio of the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the chitosan is 1: 1.
further, in the step 1), the mass ratio of methanol to ammonia water in the mixed solution of methanol and ammonia water is 7: 3; sequentially washing by distilled water, methanol and ether, and drying for 12-24 h at 20-25 ℃ in vacuum.
And further, in the step 2), adding water to dilute until the mass fraction of the linoleic acid modified chitosan in the solution is 1-2%.
Further, in the step 2), the water-soluble skin conditioner is one or more of schizophyllan, glucan, aloe vera extract, kapok extract, distiller's grains extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide; the oil is one or more of squalene, squalane, jojoba oil, sunflower seed oil, macadamia nut seed oil, tocopherol acetate, Pelargonium graveolens oil, Prinsepia utilis oil, Juniperus chinensis fruit oil and ginger root oil.
Still further, in step 2), the volume ratio of the water phase to the oil phase is 1: 1; the vitamin A is one or more of retinol, retinal and retinoic acid; the vitamin A derivative is one or more of retinol palmitate, retinol acetate and retinol retinoic acid ester.
The second purpose of the invention is realized by adopting the following technical scheme:
an anti-wrinkle repairing composition is prepared by the preparation method of the anti-wrinkle repairing composition.
Specifically, the anti-wrinkle repair composition comprises the following raw materials in percentage by weight:
water phase: 10-20 wt% of linoleic acid modified chitosan solution, 5-10 wt% of Schizophyllum commune polysaccharide, 5-10 wt% of glucan, 5-10 wt% of aloe vera extract, 2-5 wt% of kapok extract, 2-5 wt% of distillers meal extract, 2-5 wt% of horse chestnut extract, 2-5 wt% of rehmannia root extract, 2-5 wt% of quinoa extract and 2-5 wt% of collagen peptide;
oil phase: 20-30 wt% of grease, 0.01-0.1% of vitamin A and/or vitamin A derivatives; make up to 100 wt% from water in the aqueous phase.
The third purpose of the invention is realized by adopting the following technical scheme:
a cosmetic comprises the above anti-wrinkle repairing composition as raw material. Cosmetic formulations include, but are not limited to, creams, lotions, mists, essences, masks, gels, foundations, and sprays.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the anti-wrinkle repair composition comprises the steps of firstly coupling linoleic acid (CS) and chitosan (LA) to obtain linoleic acid modified chitosan, dissolving the linoleic acid modified chitosan in an acetic acid aqueous solution to obtain colloidal particles, then dissolving the linoleic acid modified chitosan (CS-LA) colloidal particles in water, and adding a water-soluble skin conditioner to obtain a water phase; and then dissolving the vitamin A and/or the vitamin A derivative in oil to form an oil phase, mixing and emulsifying the water phase and the oil phase to obtain a CS-LA embedded vitamin A and/or vitamin A derivative Pickering emulsion, and loading the vitamin A and/or the vitamin A derivative by linoleic acid modified chitosan, so that the vitamin A and/or the vitamin A derivative can be protected from being influenced by the external environment to lose efficacy, and the release of the vitamin A and/or the vitamin A derivative can be controlled to better exert the efficacy.
(2) The chitosan and the linoleic acid are mediated by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDC), an amido bond is formed between the carboxyl of the linoleic acid and the amino of the chitosan, and a spacer molecule is not left, so that the amidated derivative of the chitosan is obtained.
(3) The anti-wrinkle repair composition mainly contains vitamin A and/or vitamin A derivatives, and can improve the softness and smoothness of skin; retinol has antioxidant effect, and can accelerate the renewal of deep skin cells, promote skin to produce more epidermal protein, make skin more elastic, and improve acne and wrinkle. And one or more than two of schizophyllan, glucan, aloe barbadensis extract, kapok extract, distiller's grains extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide are used as a water-soluble skin conditioner for compounding, so that the stimulation of vitamin A and/or vitamin A derivatives can be reduced, and the effects of oxidation resistance, wrinkle resistance, bacteriostasis and moisture preservation are achieved.
(4) The anti-wrinkle repair composition can be used as one of raw materials of cosmetics, the Pickering emulsion has better compatibility, and is suitable for most of common oil phases and preservatives in the cosmetics, and the volume fraction of an inner phase, the pH value of an aqueous phase and the salt concentration can be changed in a wider range. The Pickering emulsion has higher stability, can meet the requirement of cosmetics on long shelf life, and can be embedded with other bioactive components simultaneously for constructing multifunctional cosmetics.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The anti-wrinkle repair composition comprises the following raw materials in percentage by weight:
water phase: 10-20 wt% of linoleic acid modified chitosan solution, 5-10 wt% of Schizophyllum commune polysaccharide, 5-10 wt% of glucan, 5-10 wt% of aloe vera extract, 2-5 wt% of kapok extract, 2-5 wt% of distillers meal extract, 2-5 wt% of horse chestnut extract, 2-5 wt% of rehmannia root extract, 2-5 wt% of quinoa extract and 2-5 wt% of collagen peptide;
oil phase: 20-30 wt% of grease, 0.01-0.1% of vitamin A and/or vitamin A derivatives; make up to 100 wt% from water in the aqueous phase.
The Schizophyllum commune polysaccharide and glucan are both derived from mushrooms and have important effects in resisting inflammation, ultraviolet rays and oxidation. The promotion effect of the collagen peptide on the growth of fibrin, the inhibition of elastin, the synthesis of collagen and the removal effect of free radicals show that the collagen peptide has good skin-activating and anti-aging effects; has effects in promoting cholesterol synthesis, changing sebum composition, reducing gloss, and improving skin softness; it also has antibacterial, antiinflammatory and moisturizing effects. The common bombax flower extract contains flavone, has strong antibacterial, lipid reducing, skin caring and skin aging preventing effects, has strong skin penetration, can reach deep skin, and can inhibit hyaluronidase activity, prolong the activity of the product, eliminate free radicals, and absorb ultraviolet ray, so as to inhibit and eliminate skin mottle.
The distiller's grains extract has excellent bactericidal and bacteriostatic effects, and has anti-inflammatory, androgen secretion inhibiting and antioxidant effects. The horse chestnut extract has the functions of clearing away heat and toxic materials, cooling blood, relieving swelling, clearing heat and promoting diuresis, and can be used for treating acne, furuncle, hemorrhoid, etc. The rehmannia root extract has the functions of activating skin and resisting aging, and can be used for anti-aging cosmetics. And has better moisture retention capability. The quinoa extract has effects of promoting collagen production, inhibiting elastase activity, resisting wrinkle, and resisting aging; promoting hyaluronic acid production in cells, and can be used as humectant; in addition, the composition has the effects of inhibiting the generation of androgen dihydrotestosterone, and preventing and treating diseases caused by high androgen, such as acne and alopecia. The Aloe Barbadensis Miller extract has antibacterial, antioxidant, antiinflammatory, and antiallergic effects, and has effects of preventing allergy, keeping moisture, preventing and treating acne, and resisting aging.
The compositions of examples 1 to 5 are shown in Table 1.
TABLE 1 formulation of the compositions of examples 1-5
Wherein the grease used in the embodiment 1 is mixed by mass ratio of 1: 1: 1 squalane, macadamia nut seed oil and juniper berries oil; the mass ratio of the grease used in example 2 was 1: 1: 1 jojoba oil, sunflower seed oil, macadamia nut seed oil; the mass ratio of the grease used in example 3 was 1: 1 squalane and tocopheryl acetate; the mass ratio of the grease used in example 4 was 1: 1: 1: 1, prinsepia utilis royle oil, sunflower seed oil, juniper berries oil and ginger root oil; the oil used in example 5 was squalene.
The preparation method of the anti-wrinkle repair composition comprises the following steps:
1) dissolving 1g of chitosan in 100mL of 1% acetic acid aqueous solution, adding 100mL of methanol solution for dilution, adding 0.95g of linoleic acid into the solution, stirring for 5min at 20-25 ℃, dropwise adding 15mL of 0.05 g/L1-ethyl- (3-dimethylaminopropyl) carbodiimide (EDC) methanol solution, reacting for 24h at 20-25 ℃, and pouring the reaction mixture into a reactor with a mass ratio of 7: 3, stirring and filtering the mixed solution of methanol and ammonia water, taking a precipitate, sequentially washing the precipitate by distilled water, methanol and ether, and drying the precipitate in vacuum at the temperature of between 20 and 5 ℃ for 12 hours to obtain solid granular linoleic acid modified chitosan; wherein, the molar ratio of the 1-ethyl- (3-dimethylaminopropyl) carbodiimide to the chitosan is equal to about 1: 1;
2) diluting the linoleic acid modified chitosan with water to the concentration of 1%, stirring until the content is completely dispersed to obtain a linoleic acid modified chitosan solution, and then adding a water-soluble skin conditioner and water to obtain a water phase;
3) dissolving vitamin A and/or vitamin A derivatives in oil to obtain oil phase;
4) mixing the components in a volume ratio of 1: 1, mixing the water phase and the oil phase, and emulsifying for 5min at the rotating speed of 2200r/min by a high-speed shearing machine to obtain the linoleic acid modified chitosan embedded vitamin A and/or vitamin A derivative Pickering emulsion, namely the anti-wrinkle repair composition.
Comparative example 1
Comparative example 1 differs from example 1 in that: comparative example 1 no linoleic acid modified chitosan was added and the water soluble skin conditioning agent and the levels of oil and retinol were the same as in example 1.
The preparation method of comparative example 1 includes the following steps:
1) adding deionized water and a water-soluble skin conditioner in a water phase into a water phase pot, adding an acryloyl dimethyl ammonium taurate/VP copolymer (surfactant), and stirring until the components are uniformly dispersed to obtain a water phase;
2) adding SEPLGEL 305 and polydimethylsiloxane (emulsifier) into an emulsifying pot, adding oil and retinol to obtain an oil phase, pumping the water phase into the emulsifying pot, and mixing the oil phase and the water phase to obtain an emulsion.
Comparative example 2
Comparative example 2 differs from example 1 in that: the chitosan of comparative example 1 was not modified with linoleic acid. Directly preparing a chitosan solution with the concentration of 1 percent as an emulsifier.
Comparative example 3
Comparative example 3 differs from example 1 in that; no water-soluble skin conditioning agent was added to the aqueous phase of comparative document 3.
Evaluation of Effect and test
In vitro DPPH free radical scavenging experiment
Preparation of DPPH free radical solution: weighing a certain amount of DPPH free radical powder, dissolving with absolute ethyl alcohol, fixing the volume to 500mL, and preparing into a solution with the concentration of 2 x 10-3mol/L as mother liquor (stored in dark place), diluted to a concentration of 0.8X 10-4The initial reaction concentration of the DPPH solution is mol/L.
Preparing a sample solution: weighing 1g of the freeze-dried powder obtained in the embodiments 1-5 and the comparative examples 1-7 and the emulsion obtained in the comparative example 8, and adding the weighed freeze-dried powder and the emulsion into 20mL of pure water to obtain 14 groups of sample solutions respectively.
The test method comprises the following steps: taking 2mL of sample solution and 2.5mL of LDPPH free radical solution As sample groups, adding the sample groups into a 5mL centrifuge tube, shaking up, sealing and standing for 20min at room temperature, and measuring the absorbance value at the wavelength of 517nm and recording As; taking a mixed solution of X mL of a blank solvent and 2.5mL of DPPH free radicals as a control group, and measuring the absorbance value as Ac; taking a mixed solution of X mL of sample and 2.5mL of absolute ethyl alcohol as a blank set, and measuring the absorbance value as Ab; the volume of the solution was adjusted to zero with 50% ethanol, and ascorbic acid (Vc) was used as a positive control.
The DPPH free radical removing capacity of the sample is calculated according to a formula (1), and the in-vitro antioxidant capacity of the sample is inspected by taking the DPPH free radical removing capacity as an index.
In the formula: as: absorbance of (sample solution + DPPH radical solution); ac: absorbance of (sample solvent + DPPH radical solution); ab: (sample solution + absolute ethanol solution).
DPPH radical clearance assay for each group: respectively preparing mother liquor of each medicine extract and 0.2g/L mother liquor of ascorbic acid (Vc). Diluting the mother liquor of each medicine into a series of concentrations, and measuring the DPPH free radical clearance of samples with each concentration. Specific data are shown in table 1.
TABLE 1 DPPH radical scavenging Rate for each set of sample solutions
Group of | Clearance rate% |
Example 1 | 95.63 |
Example 2 | 93.15 |
Example 3 | 94.27 |
Example 4 | 91.52 |
Example 5 | 90.47 |
Comparative example 1 | 94.56 |
Comparative example 2 | 76.19 |
Comparative example 3 | 82.39 |
As can be seen from table 1, example 1 is the most preferred example, and comparative example 3 has significantly reduced antioxidant effect due to the absence of added water-soluble skin conditioner, so that the compounding of schizophyllan, dextran, aloe vera extract, kapok extract, distillers meal extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide with vitamin a or vitamin derivatives can improve the antioxidant effect. The antioxidant ability of comparative example 1 is lower than that of example 1, because the present invention wraps vitamin a and/or vitamin a derivatives in Pickering emulsion to protect and slowly release vitamin a and/or vitamin a derivatives, the anti-aging effect of example 1 is good. In contrast, in comparative example 2, since the unmodified chitosan solution was added, the solution had no emulsifying ability, and the emulsion of comparative example 2 was very poor in the stability and was very likely to cause delamination.
Two or more skin irritation tests
The inspection basis is as follows: safety technical Specification for cosmetics (2015 year edition)
The preparation method of the test substance comprises the following steps: the test was performed directly with the stock solution.
Experimental groups: emulsions of example 1, comparative example 1 and comparative example 2
Experimental animals: healthy common-grade New Zealand rabbits with the weight of 2.0-2.6 kg are selected.
The test results are shown in table 2.
TABLE 2 multiple skin irritation test results for each group of emulsions
As can be seen from table 2, the emulsion of comparative example 1, which was prepared by a conventional mixing and stirring method, did not exhibit sustained release, and retinol directly entered the skin in large amounts after being absorbed in the outer aqueous phase, resulting in irritation. The emulsion of comparative example 2 was not emulsified due to the unmodified chitosan, and the emulsion was very stratified, so that retinol was directly contacted with the skin, causing severe irritation. In the embodiment 1, the linoleic acid modified chitosan embedded vitamin A and/or vitamin A derivative Pickering emulsion can slowly release the retinol, reduce the irritation of the retinol and improve the safety and the stability.
Third, moisture retention test
The test method comprises the following steps: 5.0g of each of the compositions of examples 1 to 5 and comparative examples 1 to 3 was weighed, placed in weighing bottles, and placed in an environment having a relative humidity of 43% and 81% at room temperature (24 to 30 ℃) for 24 hours, and the moisture retention rate was calculated according to formula (1).
In the formula, m0G, the mass of a sample to be detected; m isnFor the sample after being placed for 24 hoursMass, g.
The moisturizing rate data for each group is shown in table 1.
TABLE 3 moisture retention data for each group
As can be seen from Table 3, examples 1 to 5 all have good moisturizing effects, and comparative example 3 does not contain a water-soluble skin conditioner, so that the moisturizing effect is reduced, which shows that the compounding of ceramide, plant soothing extract and polyol has good moisturizing effects. Comparative example 1 the conventional preparation method of mixing the components with water was used, so that the ceramide dispersibility was not good, affecting the moisturizing effect.
Fourth, testing bacteriostatic property
The samples of example 1 and comparative examples 1-3 were tested for their inhibitory effect against Propionibacterium acnes and Staphylococcus epidermidis, and the data are shown in Table 4. Setting positive control group and blank group (20% ethanol)
TABLE 4 bacteriostatic anti-inflammatory data for example 1 and comparative examples 1-3
As can be seen from Table 4, example 1 has an obvious inhibitory effect on the inhibitory zone of Staphylococcus epidermidis and Propionibacterium acnes, which indicates that the bacteriostatic acne-resisting agent has an obvious bacteriostatic and anti-acne effect. In the comparative example 3, the plant soothing component is not added, so that the bacteriostatic performance is reduced, while the emulsion in the comparative example 2 cannot perform an emulsifying effect due to the unmodified chitosan, so that the emulsion is seriously layered, and the bacteriostatic effect is reduced. The emulsion of comparative example 1 is prepared by a conventional mixing and stirring method, and although the slow release effect cannot be achieved, the bacteriostatic effect is affected. Therefore, the invention has good bacteriostatic and anti-acne effects by compounding the ceramide, the plant soothing extract and the polyalcohol.
Fifth, wrinkle-removing effect test
Volunteer selection criteria: 20 volunteers aged 30-35 years randomly selected skin of 1cm multiplied by 1cm on the left face or the right face as a test group and skin around the other face as a blank group according to a random double-blind principle. 20 volunteers were divided into 4 groups, and the compositions of example 1 and comparative examples 1 to 3 were used, respectively.
2) The volunteers were administered the corresponding composition 1 time each day in the morning and evening (test group, blank group with skin care product without test group ingredients) for 8 weeks without co-administration with other wrinkle-removing skin care products during the test period.
3) Visits were 1 at 0, 2, 4 and 8 weeks for 4 total. Before each test, a subject needs to clean the face with clean water, wipe the face water with a paper towel without fluorescent agent, sit still for at least 20min in a constant temperature and humidity environment (20-22 ℃ and 40-60% of relative humidity), and measure by a measurer.
4) The instrument test method comprises the following steps: wrinkle skin locations around the volunteer's left and right eyes were measured using the rapid three-dimensional imaging system Primos for skin and wrinkle volumes were recorded (see table 5).
TABLE 5 wrinkle volume data after application of compositions of example 1 and comparative examples 1-3
The wrinkle volume value represents the volume of wrinkles in the analysis area, and the lower the index value, the smaller the wrinkle volume and the fewer wrinkles. The wrinkle volume values of the volunteers were measured using a skin rapid three-dimensional imaging system, and the results are shown in table 5, in which the wrinkle volume value was the highest at week 0 of the test group and showed a gradually decreasing trend after 2, 4 and 8 weeks by using each group of eye creams; the wrinkle removing effect of the composition of the invention is the best in example 1, and the wrinkle volume improving value is the smallest in comparative example 3 because no plant soothing component is added, which shows that the composition of the invention has better effects of improving skin elasticity and removing wrinkles through the compounding of various effective components. The emulsion of the comparative example 2 cannot perform an emulsifying function due to the unmodified chitosan, and the emulsion is seriously layered, so that the acne removing effect is reduced. The emulsion of comparative example 1, which is prepared by a conventional mixing and stirring method, cannot exhibit a sustained-release effect and has a reduced wrinkle-removing effect.
Sixthly, stability test
The compositions of example 1 and comparative examples 1 to 3 were subjected to a stability test by placing 10g of each of the compositions in a test tube, sealing the test tube, heating the test tube in a water bath at 50 ℃ for 30 days, and observing changes in the appearance of the test tube; another sample was irradiated with a cold color fluorescent lamp at room temperature at an illumination intensity of 2000Lux, and the change in appearance was observed, with the results shown in table 6.
TABLE 6 appearance change data for each group
As can be seen from Table 6, the product of the present invention has higher stability by making it into Pickering emulsion.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. The preparation method of the anti-wrinkle repair composition is characterized by comprising the following steps:
1) mixing linoleic acid and chitosan for coupling to obtain linoleic acid modified chitosan;
2) diluting the linoleic acid modified chitosan with water to obtain a linoleic acid modified chitosan solution, and then adding a water-soluble skin conditioner and water to obtain a water phase;
3) dissolving vitamin A and/or vitamin A derivatives in oil to obtain oil phase;
4) mixing and emulsifying the water phase and the oil phase to obtain linoleic acid modified chitosan embedded vitamin A and/or vitamin A derivative Pickering emulsion, namely the anti-wrinkle repair composition.
2. The method for preparing an anti-wrinkle repair composition according to claim 1, wherein in step 1), the chitosan is dissolved in an aqueous acetic acid solution to obtain a chitosan solution, then linoleic acid is added, a methanol solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is added at 20 to 25 ℃ under stirring, after the reaction, the reaction mixture is added to a mixed solution of methanol and ammonia water under stirring, and the mixture is filtered, and the precipitate is taken out, washed, and dried to obtain the solid linoleic acid modified chitosan.
3. The method for preparing the anti-wrinkle repair composition according to claim 1 or 2, wherein in step 1), the mass ratio of the chitosan to the linoleic acid is 1: (0.8 to 1); the molar ratio of the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the chitosan is 1: 1.
4. the method for preparing an anti-wrinkle repair composition according to claim 2, wherein in step 1), the mass ratio of methanol to ammonia water in the mixed solution of methanol and ammonia water is 7: 3; sequentially washing by distilled water, methanol and ether, and drying for 12-24 h at 20-25 ℃ in vacuum.
5. The method for preparing the anti-wrinkle repair composition according to claim 1, wherein in the step 2), the water is added to dilute the composition until the mass fraction of the linoleic acid modified chitosan in the solution is 1-2%.
6. The method for preparing the anti-wrinkle repair composition according to claim 1, wherein in step 2), the water-soluble skin conditioner is one or more of schizophyllan, dextran, aloe vera extract, kapok extract, distillers meal extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide; the oil is one or more of squalene, squalane, jojoba oil, sunflower seed oil, macadamia nut oil, tocopherol acetate, Pelargonium graveolens oil, Prinsepia utilis oil, Juniperus chinensis fruit oil and ginger root oil.
7. The method for preparing an anti-wrinkle repair composition according to claim 1, wherein the volume ratio of the water phase to the oil phase in step 2) is 1: 1; the vitamin A is one or more of retinol, retinal and retinoic acid; the vitamin A derivative is one or more of retinol palmitate, retinol acetate and retinol retinoic acid ester.
8. An anti-wrinkle restoration composition, characterized by being prepared by the method for preparing an anti-wrinkle restoration composition according to any one of claims 1 to 7.
9. The anti-wrinkle repair composition according to claim 8, comprising the following raw materials in weight percent:
water phase: 10-20 wt% of linoleic acid modified chitosan solution, 5-10 wt% of Schizophyllum commune polysaccharide, 5-10 wt% of glucan, 5-10 wt% of aloe vera extract, 2-5 wt% of kapok extract, 2-5 wt% of distillers meal extract, 2-5 wt% of horse chestnut extract, 2-5 wt% of rehmannia root extract, 2-5 wt% of quinoa extract and 2-5 wt% of collagen peptide;
oil phase: 20-30 wt% of grease, 0.01-0.1% of vitamin A and/or vitamin A derivatives; make up to 100 wt% from water in the aqueous phase.
10. A cosmetic characterized by using the anti-wrinkle repair composition according to claim 8 or 9 as a raw material.
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