CN114652636B - 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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- CN114652636B CN114652636B CN202210233396.9A CN202210233396A CN114652636B CN 114652636 B CN114652636 B CN 114652636B CN 202210233396 A CN202210233396 A CN 202210233396A CN 114652636 B CN114652636 B CN 114652636B
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Classifications
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A—HUMAN NECESSITIES
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- 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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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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- A—HUMAN NECESSITIES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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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
- A61K8/9783—Angiosperms [Magnoliophyta]
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Abstract
The invention discloses an anti-wrinkle repair composition, a preparation method thereof and a cosmetic containing the composition, wherein the preparation method of the anti-wrinkle repair composition comprises the steps of firstly preparing colloid granular linoleic acid modified chitosan, dissolving the obtained linoleic acid modified chitosan 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 grease to form an oil phase, mixing and emulsifying the water phase and the oil phase to obtain Pickering emulsion, and loading the vitamin A and/or the vitamin A derivative by the linoleic acid modified chitosan, so that the vitamin A and/or the vitamin A derivative can be prevented from being influenced by external environment to fail, and the release of the vitamin A and/or the vitamin A derivative can be controlled to better play a role. The composition can be used as one of raw materials of cosmetics, and 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 known as retinol, which is an essential vitamin for keeping skin epithelial tissue healthy, but contains more unsaturated bonds in the structure, so vitamin a is very sensitive to visible light, ultraviolet light, oxygen, etc. The application of retinol in cosmetic formulations is also limited (such as retinol is easily oxidized in air, easily inactivated under ultraviolet irradiation, insoluble in water, etc.), and the irritation and instability of retinol limit the addition amount of retinol in cosmetics, and simultaneously lead to the failure of excellent efficacy of retinol such as anti-aging and acne removal.
In order to improve the solubility, stability and permeability of vitamin a to increase its bioavailability, vectorization techniques are widely used for embedding nutrients. Several nanocarrier systems have been popular in recent years, such as liposomes, micelles, nanoemulsions, nanoparticles, and the like. The liposome is a spherical vesicle formed by one or more phospholipid bilayer layers, and can be used for embedding a water-soluble active substance in an inner water phase, and embedding a lipid-soluble substance in the bilayer layers, wherein phospholipid molecules are susceptible to oxidative degradation caused by light, high temperature, oxygen and pH. Micelles or microemulsions are colloidal particles having a hydrophobic core and a hydrophilic surface, spontaneously formed by a surfactant in an aqueous phase when exceeding a Critical Micelle Concentration (CMC), and have a high specific surface area and a low interfacial tension due to their extremely small size, exhibiting high stability. However, a large amount of small molecular surfactant is used in the preparation of the microemulsion, and the high concentration of the surfactant can generate hemolytic toxicity, so that the application of the microemulsion often has potential safety hazards.
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, so as to obtain Pickering emulsion, and the effect of protecting and slowly releasing the vitamin A and/or the vitamin A derivatives can be achieved while the addition amount of a surfactant is reduced; it is another object of the present invention to provide an anti-wrinkle repair composition which can reduce the irritation of vitamin a and/or a vitamin a derivative, and has improved stability and safety of vitamin a and/or a vitamin a derivative; the third object of the present invention is to provide a cosmetic, which is prepared from one of the raw materials, and which has a wide applicability.
One of the purposes of the invention is realized by adopting the following technical scheme:
a method of preparing an anti-wrinkle repair composition comprising the steps of:
1) Mixing linoleic acid and chitosan for coupling to obtain solid granular linoleic acid modified chitosan;
2) Adding water into linoleic acid modified chitosan to dilute 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 derivative in oil to obtain oil phase;
4) Mixing and emulsifying the water phase and the oil phase to obtain the chitosan embedded vitamin A modified by linoleic acid and/or vitamin A derivative Pickering emulsion, namely the anti-wrinkle repair composition.
Further, in the step 1), the chitosan is dissolved in an acetic acid aqueous solution to obtain a chitosan solution, then linoleic acid is added, a methanol solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is added under stirring at 20-25 ℃, after the reaction, the reaction mixture is added into a mixed solution of methanol and ammonia water to be stirred, the mixture is filtered, a precipitate is taken, and after washing, the solid linoleic acid modified chitosan is obtained after drying.
Still further, in step 1), the mass ratio of the chitosan to the linoleic acid is 1: (0.8-1); 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 the methanol to the ammonia in the mixed solution of the methanol and the ammonia is 7:3, a step of; sequentially washing with distilled water, methanol and diethyl ether, and vacuum drying at 20-25 ℃ for 12-24 h.
In step 2), water is added to dilute the solution until the mass fraction of the linoleic acid modified chitosan is 1-2%.
Further, in the step 2), the water-soluble skin conditioner is one or more than two of schizophyllan, glucan, aloe vera extract, kapok extract, wine dreg 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, tocopheryl acetate, geranium oil, prinsepia utilis oil, juniper berry oil and ginger root oil.
Still further, in step 2), the volume ratio of the aqueous phase to the oil phase is 1:1, a step of; the vitamin A is one or more than two of retinol, retinaldehyde and retinoic acid; the vitamin A derivative is one or more than two 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 repair composition is prepared by the preparation method of the anti-wrinkle repair composition.
Specifically, the anti-wrinkle repair composition comprises the following raw materials in percentage by weight:
aqueous phase: 10 to 20 weight percent of linoleic acid modified chitosan solution, 5 to 10 weight percent of schizophyllan, 5 to 10 weight percent of glucan, 5 to 10 weight percent of aloe vera extract, 2 to 5 weight percent of kapok extract, 2 to 5 weight percent of wine dreg extract, 2 to 5 weight percent of horse chestnut extract, 2 to 5 weight percent of rehmannia root extract, 2 to 5 weight percent of quinoa extract and 2 to 5 weight percent of collagen peptide;
an oil phase: 20 to 30 weight percent of grease and 0.01 to 0.1 percent of vitamin A and/or vitamin A derivative; 100wt% is made up by 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. The cosmetic formulations include, but are not limited to, creams, lotions, aquas, essences, facial 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 coupling linoleic acid (CS) with chitosan (LA) to obtain linoleic acid modified chitosan, dissolving the linoleic acid modified chitosan (CS-LA) in an acetic acid aqueous solution to obtain colloidal particles, 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 grease to form an oil phase, mixing and emulsifying the water phase and the oil phase to obtain CS-LA embedded vitamin A and/or vitamin A derivative Pickering emulsion, and loading the vitamin A and/or the vitamin A derivative by the linoleic acid modified chitosan, so that the vitamin A and/or the vitamin A derivative can be protected from being influenced by external environment to fail, and the release of the vitamin A and/or the vitamin A derivative can be controlled more, so that the vitamin A and/or the vitamin A derivative can play a role better.
(2) The chitosan and linoleic acid of the invention are mediated by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDC), an amide bond is formed between carboxyl of linoleic acid and amino of chitosan, and no spacer molecule is left, thus obtaining amidated derivatives of chitosan.
(3) The main components of the anti-wrinkle repair composition are vitamin A and/or vitamin A derivatives, so that the softness and smoothness of skin can be improved; retinol has antioxidant effect, can accelerate the renewal speed of deep cells of skin, promote the skin to produce more epidermis protein, make the skin more elastic, and has good effect on improving acne and wrinkle. And one or more than two of schizophyllan, glucan, aloe vera extract, kapok extract, wine dreg extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide are used as 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 antioxidation, crease resistance, bacteriostasis and moisture preservation are also achieved.
(4) The anti-wrinkle repair composition can be used as one of raw materials of cosmetics, the Pickering emulsion has better compatibility, is suitable for most of common oil phases and preservatives in cosmetics, and the volume fraction of the internal phase, the pH value of the water phase and the salt concentration can be changed in a wider range. The Pickering emulsion has higher stability, can meet the requirement of long shelf life of cosmetics, and can be used for embedding other bioactive components at the same time to construct multifunctional cosmetics.
Detailed Description
The present invention will be further described with reference to the following specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
The anti-wrinkle repair composition provided by the invention comprises the following raw materials in percentage by weight:
aqueous phase: 10 to 20 weight percent of linoleic acid modified chitosan solution, 5 to 10 weight percent of schizophyllan, 5 to 10 weight percent of glucan, 5 to 10 weight percent of aloe vera extract, 2 to 5 weight percent of kapok extract, 2 to 5 weight percent of wine dreg extract, 2 to 5 weight percent of horse chestnut extract, 2 to 5 weight percent of rehmannia root extract, 2 to 5 weight percent of quinoa extract and 2 to 5 weight percent of collagen peptide;
an oil phase: 20 to 30 weight percent of grease and 0.01 to 0.1 percent of vitamin A and/or vitamin A derivative; 100wt% is made up by water in the aqueous phase.
Wherein, schizophyllan and glucan are both derived from mushroom, and have important functions in anti-inflammation, ultraviolet resistance, antioxidation and the like. The collagen peptide has the promotion effect on the growth of fibrin, the inhibition on elastin, the synthesis of collagen and the removal effect on free radicals, which shows that the collagen peptide has good skin-activating and anti-aging effects; has effects in promoting cholesterol synthesis, changing sebum composition, reducing oil gloss, and increasing skin smoothness; meanwhile, the product has antibacterial, antiinflammatory and moisturizing effects. The kapok extract contains flavone, has strong antibacterial, lipid-reducing and skin-beautifying effects and can prevent skin aging, has strong penetrability to skin, can reach deep skin, can inhibit the activity of hyaluronidase, can prolong the activity of the substance by being used together with the hyaluronidase, can eliminate free radicals, and has the function of ultraviolet absorption, so that skin color spots can be inhibited and eliminated.
The extract has good bactericidal and bacteriostatic effects, and combines anti-inflammatory, androgen secretion inhibition and antioxidant properties. The horse chestnut extract has the functions of clearing heat and detoxicating, cooling blood and detumescence, clearing heat and promoting diuresis, and can treat acne, furuncle, hemorrhoids and the like. The rehmannia root extract has the functions of activating skin and resisting aging, and can be used for anti-aging cosmetics. And has better moisturizing capability. The quinoa extract has promotion effect on collagen generation, inhibition effect on elastase activity, and anti-wrinkle and antiaging effects; has effect in promoting hyaluronic acid production in cells, and can be used as humectant; in addition, the composition has the effects of inhibiting the generation of the androgenic dihydrotestosterone and preventing and treating diseases caused by high androgenic level, such as acne, alopecia and the like. The aloe vera extract has antibacterial, antioxidant, antiinflammatory, and antiallergic activities, and has effects of preventing allergy, keeping moisture, preventing acne, and resisting aging.
The compositions of examples 1 to 5 are shown in Table 1.
Table 1 formulations of the compositions of examples 1 to 5
Wherein the grease used in example 1 has a mass ratio of 1:1:1 squalane, macadamia nut seed oil and juniper berry oil; the grease used in example 2 was 1 in mass ratio: 1:1 jojoba oil, sunflower seed oil, macadamia nut seed oil; the grease used in example 3 was 1 in mass ratio: 1 squalane and tocopheryl acetate; the grease used in example 4 was 1 in mass ratio: 1:1:1 Prinsepia utilis royle oil, sunflower seed oil, juniper berry oil and ginger root oil; the lipid used in example 5 was squalene.
The preparation method of the anti-wrinkle repair composition comprises the following steps:
1) 1g of chitosan is dissolved in 100mL of acetic acid aqueous solution with the concentration of 1%, 100mL of methanol solution is added for dilution, 0.95g of linoleic acid is added into the solution, stirring is carried out for 5min at the temperature of 20-25 ℃, 15mL of 1-ethyl- (3-dimethylaminopropyl) carbodiimide (EDC) methanol solution with the concentration of 0.05g/L is added dropwise, reaction is carried out for 24h at the temperature of 20-25 ℃, and the reaction mixture is poured into a mass ratio of 7:3, stirring and filtering the mixed solution of methanol and ammonia water, taking a precipitate, washing the precipitate sequentially by distilled water, methanol and diethyl ether, and drying the precipitate in vacuum for 12 hours at 20-5 ℃ to obtain solid granular linoleic acid modified chitosan; wherein the molar ratio of 1-ethyl- (3-dimethylaminopropyl) carbodiimide to chitosan is about equal to 1:1, a step of;
2) Adding water into linoleic acid modified chitosan to dilute to 1% concentration, stirring until the content is completely dispersed to obtain linoleic acid modified chitosan solution, and adding water-soluble skin conditioner and water to obtain water phase;
3) Dissolving vitamin A and/or vitamin A derivative in oil to obtain oil phase;
4) The volume ratio is 1:1 and the oil phase are mixed, and emulsified for 5min at the rotating speed of 2200r/min by a high-speed shearing machine, so as to obtain the chitosan embedded vitamin A modified by linoleic acid and/or the 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 conditioner and oil and retinol levels were the same as in example 1.
The preparation method of comparative example 1 comprises the following steps:
1) Adding deionized water and a water-soluble skin conditioner in an aqueous phase into an aqueous phase pot, adding an ammonium acryloyldimethyl taurate/VP copolymer (surfactant), and stirring until the mixture is uniformly dispersed to obtain an aqueous phase;
2) Adding SEPLGEL 305 and polydimethylsiloxane (emulsifier) into emulsifying pot, adding oil and retinol to obtain oil phase, pumping water phase into emulsifying pot, and mixing oil phase and water phase to obtain emulsion.
Comparative example 2
Comparative example 2 is different from example 1 in that: the chitosan of comparative example 1 was not modified with linoleic acid. Directly preparing 1% chitosan solution as 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.
Effect evaluation and test
1. In vitro DPPH free radical scavenging experiments
Preparation of DPPH radical solution: weighing a certain amount of DPPH free radical powder, dissolving with absolute ethanol, and making into solution with volume of 500mL to obtain solution with concentration of 2×10 -3 mol/L as mother liquor (stored in dark place), diluted to a concentration of 0.8X10 -4 The mol/L was used as the initial reaction concentration of DPPH solution.
Preparing a sample solution: 1g of the lyophilized powder of examples 1 to 5 and comparative examples 1 to 7 and the emulsion of comparative example 8 were weighed and added to 20mL of pure water, to obtain 14 sets 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 into a 5mL centrifuge tube, shaking uniformly, sealing and standing for 20min at room temperature, measuring absorbance value at 517nm wavelength, and marking As; taking a mixed solution of X mL of blank solvent and 2.5mL of DPPH free radical as a control group, and measuring the absorbance value as Ac; taking X mL of a sample and 2.5mL of absolute ethyl alcohol mixed solution as a blank group, and measuring an absorbance value as Ab; zeroing with equal volume of 50% ethanol, and taking ascorbic acid (Vc) as positive control.
The DPPH free radical scavenging ability of the sample is calculated according to the formula (1), and the DPPH free radical scavenging rate is used as an index to examine the in-vitro oxidation resistance of the sample.
Wherein: as: (sample solution+dpph radical solution) absorbance; ac: (sample solvent+dpph radical solution) absorbance; ab: (sample solution+absolute ethanol solution).
DPPH radical scavenging Rate determination for each group: preparing mother liquor of each medicine extract and 0.2g/L ascorbic acid (Vc) mother liquor respectively. Diluting each medicine mother solution into a series of concentrations, and measuring DPPH free radical clearance of each concentration sample. The specific data are shown in Table 1.
Table 1 DPPH radical scavenging Rate for each group 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 because no water-soluble skin conditioner is added, so that schizophyllan, dextran, aloe vera extract, kapok extract, white spirit extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide can be compounded with vitamin a or vitamin derivatives to improve the antioxidant effect. The antioxidant capacity of comparative example 1 is lower than that of example 1 because the anti-aging effect of example 1 is good because the vitamin a and/or the vitamin a derivative is coated in the Pickering emulsion to protect and slow release the vitamin a and/or the vitamin a derivative. Whereas comparative example 2 had no emulsifying power due to the addition of the unmodified chitosan solution, the emulsion of comparative example 2 had severe delamination and poor stability.
2. Multiple skin irritation test
The test basis is as follows: cosmetic safety technical Specification (2015 year edition)
The preparation method of the test object comprises the following steps: directly testing with stock solution.
Experimental group: emulsions of example 1, comparative example 1 and comparative example 2
Experimental animals: healthy normal New Zealand rabbits with the weight of 2.0-2.6 kg are selected.
The test results are shown in Table 2.
TABLE 2 results of multiple skin irritation test of each set of emulsions
As is clear from Table 2, the emulsion of comparative example 1 was prepared by conventional mixing and stirring methods, and did not exert a slow-release effect, and retinol directly entered the skin in large amounts after the outer aqueous phase was absorbed, resulting in irritation. The emulsion of comparative example 2 was severely irritated by direct contact of retinol with the skin because the emulsion was severely delaminated because the chitosan which was not modified did not play a role in emulsification. In the embodiment 1, the linoleic acid modified chitosan embedded vitamin A and/or vitamin A derivative Pickering emulsion can slowly release retinol, so that the irritation of the retinol can be reduced, and the safety and stability are improved.
3. Moisture retention test
The testing 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 a weighing flask, and placed in an atmosphere having a relative humidity of 43% and 81% at room temperature (24 to 30 ℃) for 24 hours, and the moisture retention was calculated according to formula (1).
Wherein m is 0 G, the mass of the sample to be detected; m is m n G, sample mass after 24 hours of standing.
The moisture retention 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 effect, and comparative example 3 does not add a water-soluble skin conditioner, so that the moisturizing effect is reduced, which indicates that the ceramide of the present invention has good moisturizing effect when compounded with a plant soothing extract and a polyol. Comparative example 1 used a conventional preparation method of mixing the ingredients with water, which resulted in poor dispersibility of ceramide and an effect of moisturizing.
4. Antibacterial property test
Samples of example 1 and comparative examples 1-3 were taken for their inhibition of propionibacterium acnes and staphylococcus epidermidis and the data are presented in table 4. Positive control and blank (20% ethanol) were then set up
Table 4 antibacterial anti-inflammatory data for example 1 and comparative examples 1 to 3
As can be seen from Table 4, example 1 has an obvious inhibition effect on staphylococcus epidermidis and propionibacterium acnes, and shows that the antibacterial and anti-acne effects are obvious. In the comparative example 3, the antibacterial performance is reduced because no plant soothing component is added, while the emulsion of the comparative example 2 cannot play an emulsifying role because of the non-modified chitosan, and the emulsion is severely layered, so that the antibacterial effect is reduced. The emulsion of comparative example 1 was prepared by conventional mixing and stirring methods, and although it failed to exert a slow release effect, it also affected the bacteriostatic effect. Therefore, the invention has good antibacterial and anti-acne effects by compounding the ceramide, the plant soothing extract and the polyalcohol.
5. Wrinkle removal effect test
Volunteer selection criteria: 20 volunteers aged 30-35 years old, skin of 1cm x 1cm of left face or right face is randomly selected as a test group, and skin around the other face is selected as a blank group according to a random double-blind principle. The 20 volunteers were divided into 4 groups and the compositions of example 1 and comparative examples 1 to 3 were used, respectively.
2) Volunteers used 1 time each in the morning and evening (test group, blank group, skin care product without test group components) for 8 consecutive weeks without using other wrinkle removing skin care products during the test.
3) Follow-up 1 time at weeks 0,2,4 and 8 for a total of 4 times. Before each test, the subject needs to clean the face with clear water, uses paper towel without fluorescent agent to dry the face, and sits still for at least 20min under the constant temperature and humidity environment (20-22 ℃ and relative humidity 40-60%), and is measured by a measuring staff.
4) The instrument testing method comprises the following steps: the wrinkled skin locations around the left and right eyes of the volunteer were measured using the skin rapid three-dimensional imaging system Primos, and the wrinkled volumes were recorded (see table 5).
Table 5 wrinkle volume data after use of the compositions of example 1 and comparative examples 1-3
The wrinkle volume value of the wrinkle is indicative of the volume of the wrinkles in the analysis area, and the lower the index value, the smaller the wrinkle volume and the fewer wrinkles. The volunteer wrinkle volume values were measured using a skin rapid three-dimensional imaging system, and as shown in table 5, the wrinkle volume values at 0 week of the test group were highest, and the wrinkle volume values exhibited a gradual decrease trend by using each of the eye creams 2,4 and 8 weeks; among them, example 1 had the best wrinkle-removing effect, and comparative example 3 had the least volume improvement of wrinkle volume value due to the absence of added plant soothing ingredients, demonstrating that the composition of the present invention has better effects of improving skin elasticity and removing wrinkles by compounding various active ingredients. The emulsion of comparative example 2, however, did not have an emulsifying effect due to the non-modified chitosan, and the emulsion was severely layered, resulting in a reduced acne-removing effect. The emulsion of comparative example 1 is prepared by adopting a traditional mixing and stirring method, can not play a role in slow release and has reduced wrinkle removing effect.
6. Stability test
The compositions of example 1 and comparative examples 1 to 3 were subjected to stability test by taking 10g each of the samples of the composition in test tubes, sealing, heating in a water bath at 50℃for 30 days, and observing the change in appearance; the sample was further irradiated with a cold fluorescent lamp at room temperature at an illumination intensity of 2000Lux, and the change in appearance was observed, and the results are shown in table 6.
Table 6 appearance change data for each group
As can be seen from Table 6, the product of the invention has higher stability by being made into Pickering emulsion.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.
Claims (7)
1. A method of preparing an anti-wrinkle repair composition, comprising the steps of:
1) Mixing linoleic acid and chitosan for coupling to obtain linoleic acid modified chitosan;
2) Adding water into linoleic acid modified chitosan to dilute to obtain a linoleic acid modified chitosan solution, and then adding a water-soluble skin conditioner and water to obtain a water phase; the water-soluble skin conditioner is schizophyllan polysaccharide, glucan, aloe vera extract, kapok extract, wine dreg extract, horse chestnut extract, rehmannia root extract, quinoa extract and collagen peptide;
3) Dissolving vitamin A and/or vitamin A derivative in oil to obtain oil phase;
4) Mixing and emulsifying the water phase and the oil phase to obtain a linoleic acid modified chitosan embedded vitamin A and/or vitamin A derivative Pickering emulsion, namely the anti-wrinkle repair composition;
the anti-wrinkle repair composition comprises the following raw materials in percentage by weight:
aqueous phase: 10-20wt% of linoleic acid modified chitosan solution, 5-10wt% of schizophyllan, 5-10wt% of glucan, 5-10wt% of aloe vera extract, 2-5wt% of kapok extract, 2-5wt% of wine dreg extract, 2-5wt% of horse chestnut extract, 2-5wt% of rehmannia root extract, 2-5wt% of quinoa extract and 2-5wt% of collagen peptide;
an oil phase: 20-30wt% of grease, and 0.01-0.1% of vitamin A and/or vitamin A derivative; make up 100wt% of water in the aqueous phase;
in the step 1), chitosan is dissolved in acetic acid aqueous solution to obtain chitosan solution, then linoleic acid is added, under the condition of stirring at 20-25 ℃, methanol solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is added, after reaction, the reaction mixture is added into mixed solution of methanol and ammonia water to stir, filtration is carried out, precipitate is taken, and after washing, solid linoleic acid modified chitosan is obtained by drying.
2. The method for producing an anti-wrinkle repair composition according to claim 1, wherein in step 1), the mass ratio of the chitosan to the linoleic acid is 1: (0.8-1); the molar ratio of the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the chitosan is 1:1.
3. the method for producing an anti-wrinkle repair composition according to claim 1, wherein in step 1), the mass ratio of methanol to ammonia in the mixed solution of methanol and ammonia is 7:3, a step of; and washing with distilled water, methanol and diethyl ether in sequence, and vacuum drying at 20-25 ℃ for 12-24 hours.
4. The method for producing an anti-wrinkle repair composition according to claim 1, wherein in step 2), water is added to dilute the composition to a mass fraction of 1-2% of linoleic acid modified chitosan in the solution.
5. The method of preparing an anti-wrinkle repair composition according to claim 1, wherein in step 2), the volume ratio of the aqueous phase to the oil phase is 1:1, a step of; the vitamin A is one or more than two of retinol, retinaldehyde and retinoic acid; the vitamin A derivative is one or more than two of retinol palmitate, retinol acetate and retinol retinoic acid ester.
6. An anti-wrinkle repair composition, characterized by being prepared by the method for preparing the anti-wrinkle repair composition according to any one of claims 1 to 5.
7. A cosmetic comprising the anti-wrinkle composition according to claim 6 as a raw material.
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