Supramolecular ionic liquid polypeptide composition as well as preparation method and application thereof
By using supramolecular ionic liquid polypeptide compositions, combined with Asahi leaf polypeptide, palmitoyl tripeptide-5 and collagen peptide, the problem of poor effect of existing skin anti-aging products is solved, and the effect of significantly reducing wrinkles and firming skin is achieved, and a better skin anti-aging management solution is provided.
Patent Information
- Application Number
- CN202510208546.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-25
- Publication Date
- 2025-05-16
AI Technical Summary
Existing skin anti-aging products are difficult to effectively reduce wrinkles and firm the skin, and the direct use of Asahi leaves or their extracts is not ideal in skin care cosmetics.
A new highly efficient skin anti-aging composition is formed using a supramolecular ionic liquid composition, including a combination of L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid, combined with Asahi leaf polypeptide, palmitoyl tripeptide-5 and collagen peptide.
The composition can significantly reduce wrinkles, firm the skin, provide faster and better anti-aging effects, and has the advantages of good stability and good transdermal effect.
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Figure CN120000548A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of skin anti-aging, and in particular to a supramolecular ionic liquid protein composition and a preparation method and application thereof. Background Art
[0002] Skin is the largest organ in the human body, accounting for about 16% of body weight. It has the functions of protection, excretion, respiration, regulating body temperature and sensing external stimuli. As the first protective barrier that isolates the human body from the outside world, the skin is most susceptible to external stimuli and influences, making it more prone to aging; its intuitive symptoms include sagging skin, wrinkles, dull skin tone, dryness, enlarged pores, etc.
[0003] Although skin aging is an inevitable natural phenomenon as we age, studies have shown that proteins (such as collagen) or peptides have anti-aging effects on the skin and can alleviate or slow down the aging process to a certain extent. Collagen, in particular, has been widely used in the cosmetics field.
[0004] As people's living standards continue to improve, they pay more and more attention to their own image. In order to maintain better skin condition, they have put forward higher requirements for skin anti-aging products. Therefore, the research and development of skin anti-aging products with better anti-aging effects remains the research focus and difficulty in related fields. Summary of the invention
[0005] The purpose of the present application is to provide a novel supramolecular ionic liquid polypeptide composition and a preparation method and application thereof.
[0006] This application adopts the following technical solutions:
[0007] One aspect of the present application discloses a supramolecular ionic liquid polypeptide composition, comprising a supramolecular ionic liquid, a keiskei leaf polypeptide, palmitoyl tripeptide-5, and a collagen peptide; the supramolecular ionic liquid is a combination of a L-carnitine hydroxycitric acid ionic liquid and a betaine citric acid ionic liquid; the L-carnitine hydroxycitric acid ionic liquid has a structure shown in Formula 1, and the betaine citric acid ionic liquid has a structure shown in Formula 2;
[0008]
[0009]
[0010] It should be noted that the research in this application found that the combination of tomorrow leaf polypeptide, palmitoyl tripeptide-5, and collagen peptide, combined with a mixed supramolecular ionic liquid of L-carnitine hydroxycitrate ionic liquid and betaine citrate ionic liquid, can more effectively resist skin aging, especially in reducing wrinkles and tightening the skin, providing a new and efficient composition for skin anti-aging management.
[0011] It should also be noted that the Angelica keiskei polypeptide of the present application is a polypeptide extracted from fresh Angelica keiskei leaves and obtained by enzymatic hydrolysis. Existing studies have shown that Angelica keiskei has the effects of anti-cancer, preventing cell aging, lowering blood sugar, lowering blood pressure, protecting the liver, etc. There are also studies that directly use Angelica keiskei or Angelica keiskei extracts in cosmetics; however, the effect of directly using Angelica keiskei or Angelica keiskei extracts in skin care cosmetics is not ideal. The present application creatively discovered that the polypeptide extracted from fresh Angelica keiskei leaves and obtained by enzymatic hydrolysis, namely, Angelica keiskei polypeptide, has better skin anti-aging effects with palmitoyl tripeptide-5 and collagen peptide, and is combined with the supramolecular ionic liquid specially formulated in the present application, namely, a combination of L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid, which has a faster and better anti-aging effect.
[0012] Preferably, the supramolecular ionic liquid polypeptide composition of the present application comprises 60-70 parts by weight of supramolecular ionic liquid, 18-23 parts by weight of Angelica keiskei polypeptide, 1-2 parts by weight of palmitoyl tripeptide-5, and 11-15 parts by weight of collagen peptide.
[0013] Preferably, the collagen peptides are obtained by enzymatic hydrolysis with pepsin and trypsin.
[0014] Preferably, the weight ratio of L-carnitine hydroxycitric acid ionic liquid to betaine citrate ionic liquid is 1-5:1.
[0015] Another aspect of the present application discloses the use of the supramolecular ionic liquid polypeptide composition of the present application in the preparation of cosmetics.
[0016] Another aspect of the present application discloses a cosmetic containing the supramolecular ionic liquid polypeptide composition of the present application.
[0017] It should be noted that the cosmetics of the present application, due to the addition of the supramolecular ionic liquid polypeptide composition of the present application, have good anti-aging effects on the skin, can effectively reduce wrinkles and tighten the skin; as for the specific form of the cosmetics, it can be prepared into various forms of products according to demand, such as creams, facial masks, etc., and is not specifically limited here.
[0018] Another aspect of the present application discloses a method for preparing the supramolecular ionic liquid polypeptide composition of the present application, comprising weighing Angelica keiskei polypeptide, palmitoyl tripeptide-5, collagen peptide, L-carnitine hydroxycitrate ionic liquid and betaine citric acid ionic liquid by weight, mixing the Angelica keiskei polypeptide with the L-carnitine hydroxycitrate ionic liquid to prepare a mixed solution one, mixing the palmitoyl tripeptide-5 and the collagen peptide with the betaine citric acid ionic liquid to prepare a mixed solution two, and mixing the mixed solution one and the mixed solution two to obtain the supramolecular ionic liquid polypeptide composition of the present application.
[0019] Preferably, in the present application, the preparation method of the Angelica keiskei polypeptide includes taking the juice obtained by squeezing fresh Angelica keiskei, diluting it with water, and obtaining an Angelica keiskei solution; placing the Angelica keiskei solution in a water bath at 55-65°C for 10-40 minutes; taking it out, and after the Angelica keiskei solution is cooled to room temperature, adding trypsin and subtilisin for enzymolysis, and after the enzymolysis is completed, centrifuging and taking the supernatant; adding papain and serine protease to the supernatant and first enzymolyzing it under alkaline conditions, and after the enzymolysis is completed, centrifuging and taking the supernatant, and continuing to enzymolyze the supernatant under acidic conditions; then performing enzyme inactivation treatment on the supernatant, concentrating, and drying, to obtain the Angelica keiskei polypeptide of the present application.
[0020] Preferably, the conditions for enzymolysis with trypsin and subtilisin are: enzymolysis at pH 7.5 and temperature 37° C. for 0.5-2 h.
[0021] Preferably, papain and serine protease are first enzymatically hydrolyzed under alkaline conditions at pH 8.5 and temperature 42° C. for 0.5-2 h.
[0022] Preferably, the supernatant is further enzymatically hydrolyzed under acidic conditions at pH 5.5 and temperature 55° C. for 0.5-2 h.
[0023] Preferably, the preparation method of collagen peptide includes soaking cleaned animal skin, bones or tissues in water, heating to boiling, and treating at a constant temperature for 2-6 hours; then, cooling to 35-55°C, filtering to remove the filter residue, centrifuging the filtrate, and taking the supernatant as the collagen extract; using pepsin and trypsin to enzymatically hydrolyze the collagen extract, and after the enzymatic hydrolysis is completed, centrifuging to take the supernatant, performing enzyme inactivation treatment, concentrating, and drying it to obtain the collagen peptide.
[0024] Preferably, the centrifugation condition is 5000-8000 rpm for 10-20 min.
[0025] Preferably, the conditions for enzymatic hydrolysis of the collagen extract with pepsin and trypsin are: first enzymatic hydrolysis at pH 4-5 and temperature 37°C for 0.5-2h, then centrifugation, taking the supernatant, and enzymatic hydrolysis at pH 7.5 and temperature 37°C for 0.5-2h.
[0026] Preferably, the preparation method of L-carnitine hydroxycitric acid ionic liquid comprises: under an inert atmosphere, adding L-carnitine and hydroxycitric acid to water in a molar ratio of 1:1-3, stirring evenly, heating at 60-70°C for 15-25h; then, continuing heating and performing ultrasonic treatment for 3-6h, with the ultrasonic frequency being 20-40kHz and the power being 500-1000W; after the ultrasonic treatment, performing dialysis treatment in a dialysis bag to intercept and assemble the L-carnitine hydroxycitric acid ionic liquid into a supramolecular structure.
[0027] Preferably, the method for preparing the L-carnitine hydroxycitrate ionic liquid further comprises concentrating the dialysis product to obtain a solution with a volume of 1 / 10 to 1 / 2 of the initial volume, namely the L-carnitine hydroxycitrate ionic liquid of the present application.
[0028] Preferably, the preparation method of the betaine citrate ionic liquid comprises: adding betaine hydrochloride and sodium citrate to water at a molar ratio of 1:1-6 under a mixed atmosphere of carbon dioxide and inert gas; then, heating at 35-50° C. and stirring at a pressure of 30-60 MPa for 5-24 hours; after the reaction is completed, dialyzing the product to intercept and assemble the betaine citrate ionic liquid into a supramolecular structure;
[0029] Preferably, the method for preparing the betaine citrate ionic liquid further comprises concentrating the dialysis product to obtain a solution with a volume of 1 / 10 to 1 / 2 of the initial volume, namely the betaine citrate ionic liquid of the present application.
[0030] Preferably, the volume ratio of carbon dioxide to inert gas in the mixed atmosphere of carbon dioxide and inert gas is 85-95:5-15.
[0031] The beneficial effects of this application are:
[0032] The supramolecular ionic liquid polypeptide composition of the present application has good skin anti-aging effects, can effectively reduce wrinkles and tighten the skin; and, due to the use of supramolecular ionic liquids composed of L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid, the supramolecular ionic liquid polypeptide composition of the present application has the advantages of good stability and good transdermal effect, thus providing a new and efficient composition for skin anti-aging management. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 It is the result of the rabbit corneal epithelial cell stimulation test in the examples of the present application;
[0034] Figure 2 is the result of the human keratinocyte toxicity test in the examples of this application;
[0035] Figure 3 This is the test result of the skin moisture improvement effect in the embodiment of the present application;
[0036] Figure 4 is the test result of skin anti-aging in the examples of this application;
[0037] Figure 5 It is the test result of the skin elasticity change rate in the embodiment of the present application. DETAILED DESCRIPTION
[0038] The present application is further described in detail below through specific examples. The following examples are only used to further illustrate the present application and should not be construed as limiting the present application.
[0039] Unless otherwise specified, the materials and reagents used in the following examples can be obtained from commercial sources, and the experimental methods used in the following examples are conventional methods unless otherwise specified.
[0040] Example
[0041] The supramolecular ionic liquid polypeptide composition of this example is composed of supramolecular ionic liquid, Angelica keiskei polypeptide, palmitoyl tripeptide-5, and collagen peptide, wherein the supramolecular ionic liquid is composed of L-carnitine hydroxycitric acid ionic liquid and betaine citrate ionic liquid.
[0042] The preparation method of the supramolecular ionic liquid polypeptide composition of this example comprises:
[0043] 1. Preparation of Angelica keiskei polypeptide
[0044] Fresh tomorrow leaf is taken as raw material for squeezing, and the obtained juice is added with 2-3 times volume of pure water, stirred evenly, diluted, and tomorrow leaf solution is obtained, and placed in a 60°C water bath for 20 minutes; after the solution temperature drops to room temperature, trypsin and subtilisin are added for enzymolysis under pH 7.5, the enzymolysis time is 1 hour, the enzymolysis temperature is 37°C, centrifuged, and the supernatant is taken; papain and serine protease are added for enzymolysis under pH 8.5, the enzymolysis time is 1 hour, the enzymolysis temperature is 42°C, centrifuged, the supernatant is taken, and the pH is adjusted to 5.5 for enzymolysis for 1 hour, the enzymolysis temperature is 55°C, and after the enzymolysis is completed, the enzyme is inactivated at 90°C, concentrated, and dried to obtain tomorrow leaf polypeptide for standby use.
[0045] 2. Preparation of Collagen Peptides
[0046] The pig skin is washed with warm water, soaked in 75% ethanol for 30 seconds, taken out, rinsed with clean water, cut into pieces, boiled with water at a temperature of about 100°C, and kept boiling for 4 hours; then, cooled to a warm state, i.e., about 45°C, filtered to remove residue, centrifuged at 6000rpm for 20min, and the supernatant, i.e., collagen extract, is taken; the collagen extract is enzymatically hydrolyzed with pepsin and trypsin, specifically, pepsin and trypsin are added, first enzymatically hydrolyzed at pH 4.5 and 37°C for 1h, then centrifuged at 6000rpm for 20min, the supernatant is taken, and enzymatically hydrolyzed at pH 7.5 and 37°C for 1h; after the enzymatic hydrolysis is completed, centrifuged at 6000rpm for 20min, the supernatant is taken, and the enzyme is inactivated at 90°C, concentrated, and dried to obtain collagen peptides for standby use.
[0047] 3. Preparation of L-carnitine hydroxycitrate ionic liquid
[0048] Under the protection of nitrogen atmosphere, 0.2 mol of L-carnitine and 0.4 mol of hydroxycitric acid were added to deionized water, stirred evenly, heated to 65°C, and reacted for 16 hours; then, continued heating and ultrasonic treatment for 5 hours, with an interval of 2 seconds and 4 seconds of ultrasonic treatment, and the frequency of the ultrasound was 40kHz and the power was 1000W; after the ultrasonic treatment, dialysis treatment was performed in a dialysis bag to intercept and assemble the L-carnitine hydroxycitric acid ionic liquid into a supramolecular structure; then, the dialysis product was concentrated to obtain a solution of 1 / 3 of the initial volume, that is, the L-carnitine hydroxycitric acid ionic liquid in this example. Among them, the structural formula of the L-carnitine hydroxycitric acid ionic liquid is as follows:
[0049]
[0050] 4. Preparation of Betaine Citrate Ionic Liquid
[0051] In a mixed atmosphere of carbon dioxide and inert gas at a volume ratio of 95:5 and a gas pressure of 45 MPa, 0.1 mol of betaine hydrochloride and 0.2 mol of sodium citrate were added to 120 mL of water; then, the mixture was heated and stirred at 45°C for 12 hours; after the reaction was completed, the product was dialyzed to intercept and assemble the supramolecular structure of betaine citrate ionic liquid; the dialyzed product was concentrated to obtain a solution of 1 / 3 of the initial volume, i.e., the betaine citrate ionic liquid of this example. The structural formula of the betaine citrate ionic liquid is as follows:
[0052]
[0053] 5. Preparation of supramolecular ionic liquid polypeptide compositions
[0054] According to the formula in Table 1, weigh the Angelica keiskei polypeptide, palmitoyl tripeptide-5, collagen peptide, L-carnitine hydroxycitric acid ionic liquid and betaine citrate ionic liquid, mix the Angelica keiskei polypeptide with the L-carnitine hydroxycitric acid ionic liquid to prepare a mixed solution 1, mix the palmitoyl tripeptide-5 and the collagen peptide with the betaine citrate ionic liquid to prepare a mixed solution 2, mix the mixed solution 1 and the mixed solution 2 to obtain a supramolecular ionic liquid polypeptide composition.
[0055] Table 1 Supramolecular ionic liquid polypeptide composition formula (weight units are mg)
[0056] serial number Angelica keiskei peptide Palmitoyl Tripeptide-5 Collagen Peptides L-Carnitine Ionic Liquid Betaine Ionic Liquid Test 1 18 1 11 50 20 Test 2 23 2 15 50 10 Test 3 18 2 14 33 33 Comparison 1 18 / / 33 33 Comparison 2 / 2 14 33 33 Contrast 3 18 2 / 33 33 Contrast 4 18 / 14 33 33 Contrast 5 23 2 15 60 / Contrast 6 23 2 15 / 60 Contrast 7 23 2 15 / /
[0057] Ten supramolecular ionic liquid polypeptide compositions or polypeptide compositions were prepared according to the formula in Table 1. Control 7 used an equal amount of deionized water to replace the supramolecular ionic liquid in Test 2.
[0058] The safety and skin anti-aging performance tests of the 10 prepared supramolecular ionic liquid polypeptide compositions or polypeptide compositions were performed as follows:
[0059] Test 1 Corneal cell irritation test
[0060] The irritation caused by the composition acting on the cornea is similar to cytotoxic damage; therefore, the cytotoxicity of the composition can be reflected by detecting the degree of corneal damage. In this example, rabbit corneal epithelial cells (SIRC) were used to test the toxicity of the composition. Specifically, SIRC was contacted with the 10 supramolecular ionic liquid polypeptide compositions or polypeptide compositions in Table 1 to simulate acute corneal irritation, and the survival rate of the cells relative to those without any treatment was calculated to characterize the toxicity of the composition. The results are shown in Tables 2 and Figure 1 shown.
[0061] Table 2 Cell survival rate of corneal cell stimulation test
[0062] sample Survival rate sample Survival rate Test 1 91.5％ Contrast 3 90.9％ Test 2 91.7％ Contrast 4 90.8％ Test 3 91.2％ Contrast 5 88.6％ Comparison 1 90.8％ Contrast 6 88.2％ Comparison 2 91.2％ Contrast 7 90.7％
[0063] Table 2 and Figure 1 The results showed that the supramolecular ionic liquid polypeptide compositions or polypeptide compositions of Tests 1 to 3 and Comparisons 1 to 7 had slight stimulation to rabbit corneal epithelial cells and could meet the requirements of subsequent use.
[0064] Test 2 Human keratinocyte toxicity test
[0065] The 10 supramolecular ionic liquid polypeptide compositions or polypeptide compositions in Table 1 were added to the culture medium MEM of human keratinocytes. Specifically, 1 mL of the supramolecular ionic liquid polypeptide composition or polypeptide composition was added to every 100 mL of culture medium. The MTT model was used for detection, and the survival rate of the cells relative to those without any treatment was calculated to characterize the toxicity of the composition. The results are shown in Tables 3 and Figure 2 shown.
[0066] Table 3 Cell viability of human keratinocyte toxicity test
[0067] sample Survival rate sample Survival rate Test 1 98.3％ Contrast 3 97.6％ Test 2 97.9％ Contrast 4 98.8％ Test 3 98.1％ Contrast 5 96.5％ Comparison 1 98.7％ Contrast 6 96.8％ Comparison 2 99.1％ Contrast 7 97.1％
[0068] Table 3 and Figure 2 The results show that the toxicity of the supramolecular ionic liquid polypeptide composition or polypeptide composition of Tests 1 to 3 and Comparisons 1 to 7 to human keratinocytes is almost negligible and within the safety range.
[0069] Test 3 Skin Aging Clinical Trial
[0070] Test population: 300 people aged 25 to 55, 200 females and 100 males. All subjects had no skin diseases and were randomly selected volunteers. No specific type of people were selected or distinguished. All were tested and tested according to the same trial and testing methods.
[0071] Test method: All subjects are divided into 10 groups, and the age, gender and other factors are evenly distributed; each subject receives a 50mL serum sample, i.e., 10 supramolecular ionic liquid polypeptide compositions or polypeptide compositions in Table 1, and each group uses the same composition for testing, for example, the first group uses the supramolecular ionic liquid polypeptide composition of Test 1, the second group uses the supramolecular ionic liquid polypeptide composition of Test 2, and so on, the tenth group uses the polypeptide composition of Control 7. Usage: Apply a small amount of serum evenly on the face after cleansing every morning and evening, and use it for three months.
[0072] Before receiving the trial pack, each subject was tested for skin moisture content, skin aging grade and skin elasticity, and then the same test was performed three months later to compare the effects before use and after three months of use, so as to judge the anti-aging effects of the 10 supramolecular ionic liquid polypeptide compositions or polypeptide compositions in Table 1 on the skin.
[0073] The skin moisture content was measured by taking points on the cheek, forehead and chin of the test subject using a skin moisture tester to obtain the average value. The average value after three months of use minus the average value measured before use, and then divided by the average value measured before use × 100%, was used as the skin moisture improvement efficiency. The average value of the skin moisture improvement efficiency of each group of compositions was calculated to characterize the improvement effect of the composition on skin moisture content.
[0074] Skin aging level test uses naked eye observation for subjective evaluation. The evaluation results are divided into four levels according to the "Human Skin Aging Evaluation Standard". Specifically, first-level aging: There is no obvious depression on the face, but the skin begins to appear dull, rough, and spotted, and slight fine lines and nasolabial folds appear around the eyes; second-level aging: skin relaxation, sagging tissue, and fine wrinkles begin to deepen, such as crow's feet, forehead wrinkles, and even nasolabial folds; third-level aging: skin is obviously loose, nasolabial folds deepen, eye sockets are sunken, wrinkles deepen, facial fat is lost, and double chins may appear; fourth-level aging: 50-65 years old, facial wrinkles are more obvious, including sagging cheeks, lips and lower neck areas, thinning lips, obvious wrinkles around the mouth, etc. In order to facilitate quantitative evaluation, this example defines the score of first-level aging as 85-100 points, the score of second-level aging as 70-85 points, the score of third-level aging as 55-70 points, and the score of fourth-level aging as 10-55 points. The better the skin condition, the higher the score. The score after three months of use was subtracted from the score before use, and the result was divided by the score before use × 100% to obtain the skin anti-aging efficiency. The average skin anti-aging efficiency of each group of compositions was calculated to characterize the effect of the composition on improving skin aging.
[0075] Skin elasticity test: In this example, skin elasticity tester Corneometer MPA580 was used for detection. The larger the detection value, the better the skin elasticity. The change rate of skin elasticity before and after use was calculated, similar to the above, that is, change rate (%) = [(skin elasticity after using skin care water - skin elasticity before using skin care water) / skin elasticity before using skin care water] × 100%. The average value of the change rate of each group of compositions was calculated to characterize the improvement effect of the composition on skin elasticity.
[0076] The skin moisture content test results are shown in Table 4 and Figure 3 shown.
[0077] Table 4 Skin moisture content test results
[0078] sample Skin hydration efficiency improvement p Test 1 56％ Less than 0.05 Test 2 62％ Less than 0.05 Test 3 58％ Less than 0.05 Comparison 1 17％ Less than 0.05 Comparison 2 10％ Less than 0.05 Contrast 3 21％ Less than 0.05 Contrast 4 24％ Less than 0.05 Contrast 5 38％ Less than 0.05 Contrast 6 36％ Less than 0.05 Contrast 7 12％ Less than 0.05
[0079] Table 4 and Figure 3 The results show that the effects of experiments 1 to 3 on improving skin moisture content are significantly better than those of comparisons 1 to 7. Furthermore, compared with comparisons 5 and 6 that only use one supramolecular ionic liquid, experiments 1 to 3 that use a combination of L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid have significantly better effects on improving skin moisture content; and compared with comparison 7 that does not use supramolecular ionic liquid, the effects of comparisons 5 and 6 are significantly better. By comparing experiments 1 to 3 and comparisons 1 to 4, it can be seen that the combination of Angelica keiskei polypeptide, palmitoyl tripeptide-5, and collagen peptide in this example is significantly better than the combination of only one or two.
[0080] The skin aging test results are shown in Table 5 and Figure 4 shown.
[0081] Table 5 Skin aging test results
[0082]
[0083]
[0084] The test results of skin aging level are basically consistent with the results of skin water content improvement, that is, the skin anti-aging effects of experiments 1 to 3 are significantly better than those of comparisons 1 to 7. Experiments 1 to 3, which use a combination of two supramolecular ionic liquids, are better than comparisons 5 and 6, which use only one supramolecular ionic liquid; the combination of Angelica keiskei polypeptide, palmitoyl tripeptide-5, and collagen peptide is significantly better than the combination of only one or two of them.
[0085] The skin elasticity test results are shown in Table 6 and Figure 5 shown.
[0086] Table 6 Skin elasticity change rate test results
[0087] sample Skin elasticity change rate p Test 1 45％ Less than 0.05 Test 2 43％ Less than 0.05 Test 3 46％ Less than 0.05 Comparison 1 12％ Less than 0.05 Comparison 2 13％ Less than 0.05 Contrast 3 22％ Less than 0.05 Contrast 4 21％ Less than 0.05 Contrast 5 29％ Less than 0.05 Contrast 6 26％ Less than 0.05 Contrast 7 11％ Less than 0.05
[0088] The test results of skin elasticity change rate were basically consistent with the test results of skin aging grade and skin water content improvement, that is, the skin anti-aging effects of experiments 1 to 3 were significantly better than those of comparisons 1 to 7. Experiments 1 to 3, which combined two supramolecular ionic liquids, were better than comparisons 5 and 6, which only used one supramolecular ionic liquid; the combination of Angelica keiskei polypeptide, palmitoyl tripeptide-5, and collagen peptide was significantly better than the combination of only one or two of them.
[0089] The above test shows that the combination of Angelica keiskei polypeptide, palmitoyl tripeptide-5, and collagen peptide, and the combination of two supramolecular ionic liquids, L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid, to obtain a supramolecular ionic liquid polypeptide composition, has a good skin anti-aging effect, can effectively reduce wrinkles and tighten the skin. In addition, due to the combination of L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid, the supramolecular ionic liquid polypeptide composition has better stability and transdermal effect, so that the effects of experiments 1 to 3 are significantly better than those of comparisons 5 to 7.
[0090] The above contents are further detailed descriptions of the present application in combination with specific implementation methods, and it cannot be determined that the specific implementation of the present application is limited to these descriptions. For ordinary technicians in the technical field to which the present application belongs, several simple deductions or substitutions can be made without departing from the concept of the present application.
Claims
1. A supramolecular ionic liquid polypeptide composition, characterized in that: Including supramolecular ionic liquid, Angelica keiskei peptide, palmitoyl tripeptide-5, collagen peptide; The supramolecular ionic liquid is a combination of L-carnitine hydroxycitrate ionic liquid and betaine citrate ionic liquid; The L-carnitine hydroxycitrate ionic liquid has a structure shown in Formula 1, and the betaine citrate ionic liquid has a structure shown in Formula 2; 2. The supramolecular ionic liquid polypeptide composition according to claim 1, characterized in that: The invention comprises 60-70 parts by weight of supramolecular ionic liquid, 18-23 parts by weight of Angelica keiskei polypeptide, 1-2 parts by weight of palmitoyl tripeptide-5, and 11-15 parts by weight of collagen peptide.
3. The supramolecular ionic liquid polypeptide composition according to claim 1 or 2, characterized in that: The collagen peptides are obtained by enzymatic hydrolysis with pepsin and trypsin.
4. The supramolecular ionic liquid polypeptide composition according to claim 1 or 2, characterized in that: The weight ratio of the L-carnitine hydroxycitric acid ionic liquid to the betaine citric acid ionic liquid is 1-5:
1.
5. Use of the supramolecular ionic liquid polypeptide composition according to any one of claims 1 to 4 in the preparation of cosmetics.
6. A cosmetic comprising the supramolecular ionic liquid polypeptide composition according to any one of claims 1 to 4.
7. The method for preparing the supramolecular ionic liquid polypeptide composition according to any one of claims 1 to 4, characterized in that: The method comprises weighing Angelica keiskei polypeptide, palmitoyl tripeptide-5, collagen peptide, L-carnitine hydroxycitric acid ionic liquid and betaine citric acid ionic liquid by weight, mixing the Angelica keiskei polypeptide with the L-carnitine hydroxycitric acid ionic liquid to prepare a mixed solution one, mixing the palmitoyl tripeptide-5 and the collagen peptide with the betaine citric acid ionic liquid to prepare a mixed solution two, and mixing the mixed solution one with the mixed solution two to obtain the supramolecular ionic liquid polypeptide composition.
8. The preparation method according to claim 7, characterized in that: The preparation method of the Angelica keiskei polypeptide comprises the following steps: taking juice obtained by squeezing fresh Angelica keiskei, diluting it with water, and obtaining an Angelica keiskei solution; placing the Angelica keiskei solution in a water bath at 55-65° C. for 10-40 minutes; taking it out, and after the Angelica keiskei solution is cooled to room temperature, adding trypsin and subtilisin for enzymolysis, centrifuging it after the enzymolysis is completed, and obtaining a supernatant; adding papain and serine protease to the supernatant for enzymolysis under alkaline conditions, centrifuging it after the enzymolysis is completed, obtaining a supernatant, and further enzymolyzing the supernatant under acidic conditions; and then performing enzyme inactivation treatment on the supernatant, concentrating it, and drying it, so as to obtain the Angelica keiskei polypeptide; Preferably, the conditions for enzymolysis with trypsin and subtilisin are: enzymolysis at pH 7.5 and temperature 37° C. for 0.5-2 h; Preferably, papain and serine protease are first enzymatically hydrolyzed under alkaline conditions at pH 8.5 and temperature 42° C. for 0.5-2 h; Preferably, the supernatant is further enzymatically hydrolyzed under acidic conditions at pH 5.5 and temperature 55° C. for 0.5-2 h.
9. The preparation method according to claim 7, characterized in that: The preparation method of the collagen peptide comprises the following steps: soaking cleaned animal skin, bone or tissue in water, heating to boiling, and treating at a constant temperature for 2-6 hours; then cooling to 35-55° C., filtering to remove the filter residue, centrifuging the filtrate, and taking the supernatant as the collagen extract; enzymatically hydrolyzing the collagen extract with pepsin and trypsin, and after the enzymatic hydrolysis is completed, centrifuging to take the supernatant, performing enzyme inactivation treatment, concentrating, and drying the supernatant to obtain the collagen peptide; Preferably, the centrifugation condition is 5000-8000 rpm for 10-20 min; Preferably, the conditions for enzymatic hydrolysis of the collagen extract with pepsin and trypsin are: first enzymatic hydrolysis at pH 4-5 and temperature 37°C for 0.5-2h, then centrifugation, taking the supernatant, and enzymatic hydrolysis at pH 7.5 and temperature 37°C for 0.5-2h.
10. The preparation method according to any one of claims 7 to 9, characterized in that: The preparation method of the L-carnitine hydroxycitric acid ionic liquid comprises: adding L-carnitine and hydroxycitric acid to water in a molar ratio of 1:1-3 under an inert atmosphere, stirring evenly, heating at 60-70° C. for 15-25 hours; then, continuously heating, and performing ultrasonic treatment for 3-6 hours, wherein the ultrasonic frequency is 20-40 kHz and the power is 500-1000 W; after the ultrasonic treatment, performing dialysis treatment in a dialysis bag to intercept and assemble the L-carnitine hydroxycitric acid ionic liquid into a supramolecular structure; Preferably, the method for preparing the L-carnitine hydroxycitrate ionic liquid further comprises concentrating the dialysis product to obtain a solution with a volume of 1 / 10 to 1 / 2 of the initial volume, namely the L-carnitine hydroxycitrate ionic liquid; Preferably, the preparation method of the betaine citrate ionic liquid comprises: adding betaine hydrochloride and sodium citrate to water in a molar ratio of 1:1-6 under a mixed atmosphere of carbon dioxide and inert gas; then, heating at 35-50° C. and stirring at a pressure of 30-60 MPa for 5-24 hours; after the reaction is completed, dialyzing the product to intercept and assemble the betaine citrate ionic liquid into a supramolecular structure; Preferably, the method for preparing the betaine citrate ionic liquid further comprises concentrating the dialysis product to obtain a solution having a volume of 1 / 10 to 1 / 2 of the initial volume, namely the betaine citrate ionic liquid; Preferably, the volume ratio of carbon dioxide to inert gas in the mixed atmosphere of carbon dioxide and inert gas is 85-95:5-15.