A skin care composition and its preparation method and application

Abstract

The present invention proposes a skin care composition and a preparation method and application thereof, belonging to the technical field of cosmetics. The composition is prepared from the following raw materials by weight: 3-5 parts of glycerol glucoside, 1-2 parts of ectoine, 12-15 parts of polysaccharide composition, 0.1-0.2 parts of penetration enhancer composition, 0.3-0.5 parts of carbomer, 10-15 parts of jojoba oil, and 20-40 parts of purified water. The skin care composition prepared by the present invention has a wide source of raw materials, is safe and non-irritating, has a simple preparation method, is low in cost, has good moisturizing, reduces skin sensitivity, whitens, tightens, improves skin elasticity, has antibacterial, anti-inflammatory, and skin repair effects, and has broad application prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and in particular to a skin care composition and a preparation method and application thereof. Background Art

[0002] Modern people lead fast-paced lives, have poor sleep, lack skin care, and are increasingly polluted by the environment. Ultraviolet rays, radiation, computer and electrical radiation, smoking and drinking, excessive exercise, stress, excessive consumption of processed foods, and excessive intake of fats and oils, etc., all of these factors cause many skin problems. Skin is an important part of maintaining human life and health. It is the first barrier of the body, directly in contact with the outside world, and is easily affected by environmental factors and causes damage. As the environment continues to deteriorate and human pollution sources continue to increase, the skin has become more sensitive to the harsh external environment. Human skin is a barrier between the body and the environment. It is the organ that has the longest contact time with the outside world and the largest area exposed to the air. Therefore, environmental air pollution is an important risk factor for skin diseases.

[0003] Chinese invention patent CN103735458B discloses a skin anti-allergic repair composition, which contains, by weight percentage: 5%-12% moisturizer, 0.1%-3.0% thickener, 1%-4% skin repair agent, 0.1%-1.5% preservative, and water balance. The skin anti-allergic repair composition of the invention has strong effects of clearing away heat and detoxification, anti-allergic repair, anti-inflammatory and astringent; other auxiliary added components are selected to make the skin tender, smooth, moisturizing and mild and non-irritating to the skin. Moisturizers, preservatives, thickeners, etc. are easy to use, and can achieve the purpose of moisturizing, anti-inflammatory and itching, and repairing damaged skin. It is suitable for sensitive skin and skin allergies, itching, desquamation, redness, swelling, red bloodshot and other phenomena caused by improper use of cosmetics. However, the existing skin care compositions are mainly aimed at people who have suffered from environmental pollution and have skin sensitivity, and are not compositions for defending against environmental pollution.

[0004] Chinese patent application CN104398435A discloses a mild exfoliating mask, comprising the following components in percentage by weight: 0.5-1.0% fruit acid, 0.03-3% grape seed oil, 0.02-2% ginsenoside, 0.01-1% diosgenin, 4-10% volcanic mud, 5-10% glycerol, 2-4% propylene glycol, 0.05-2% salicylic acid, 20-40% kaolin, and the balance is deionized water. Fruit acid and salicylic acid are used in Chinese patent application CN104398435A. We know that the two major factors that determine the effects of fruit acid and salicylic acid are concentration and pH value, and the effects of fruit acid and salicylic acid will be weakened due to too low concentration or too high pH value. However, the salicylic acid used in Chinese patent application CN104398435A has very low solubility in water, which will reduce the exfoliating effect of the exfoliating mask. In addition, insoluble salicylic acid will cause certain irritation to skin with skin lesions and sensitive skin, and will also affect the stability of the formula system.

[0005] Therefore, there is a strong demand for skin care compositions that can enhance the skin's self-repairing ability and enable the skin to repair itself in a healthier environment. Summary of the invention

[0006] The purpose of the present invention is to provide a skin care composition and its preparation method and application, which has a wide source of raw materials, is safe and non-irritating, has a simple preparation method, is low in cost, has good moisturizing, reduces skin sensitivity, whitens, tightens, improves skin elasticity, has antibacterial and anti-inflammatory effects, and can repair skin, and has broad application prospects.

[0007] The technical solution of the present invention is achieved in this way:

[0008] The present invention provides a skin care composition, which is prepared from the following raw materials by weight: 3-5 parts of glyceryl glucoside, 1-2 parts of ectoine, 12-15 parts of a polysaccharide composition, 0.1-0.2 parts of a penetration enhancer composition, 0.3-0.5 parts of carbomer, 10-15 parts of jojoba oil, and 20-40 parts of purified water;

[0009] The penetration enhancer composition is composed of alkyl-substituted ursolic acid bornyl and menthol, with a mass ratio of 12-15:2-4;

[0010] The structural formula of the alkyl-substituted ursolic acid bornyl ester is shown in Formula I:

[0011]

[0012] Wherein, R = C6-C12 alkyl chain;

[0013] The polysaccharide composition consists of traditional Chinese medicine polysaccharide, algae polysaccharide and hyaluronic acid, and the mass ratio is 7-10:3-5:1-2.

[0014] As a further improvement of the present invention, the preparation method of the alkyl-substituted ursolic acid bornyl ester is as follows:

[0015] S1. reacting ursolic acid and borneol to obtain ursolic acid borneol ester;

[0016] S2. reacting ursolic acid bornyl ester with an alkyl halide to obtain an alkyl-substituted ursolic acid bornyl ester.

[0017] As a further improvement of the present invention, the molar ratio of ursolic acid to borneol in step S1 is 1.1-1.2:1, the reaction temperature is 100-120°C, and the time is 6-8h; the molar ratio of ursolic acid borneol ester and alkyl halide in step S2 is 1.1-1.2:1, the reaction temperature is 50-60°C, and the time is 1-3h, and the alkyl halide is selected from at least one of 1-chlorohexane, 1-bromohexane, 1-chloroheptane, 1-bromoheptane, 1-chlorooctane, 1-bromooctane, 1-chlorononane, 1-bromononane, 1-chlorodecane, 1-bromodecane, 1-chloroundecane, 1-bromodecane, 1-chlorododecane, and 1-bromododecane.

[0018] As a further improvement of the present invention, the preparation method of the alkyl-substituted ursolic acid bornyl ester is as follows:

[0019] S1. Add 1.1-1.2 molar equivalents of ursolic acid and 1 molar equivalent of borneol to toluene, add 3-5wt% of concentrated sulfuric acid to the total mass of the system, heat to reflux for 6-8h, cool to room temperature, filter, wash, and dry to obtain ursolic acid borneol ester;

[0020] S2. Add 1.1-1.2 molar equivalents of ursolic acid bornyl ester and 3-5 molar equivalents of triethylamine to acetonitrile, add 1 molar equivalent of alkyl halide, heat to 50-60°C, stir to react for 1-3h, cool to room temperature, filter, wash, and recrystallize from ethyl acetate to obtain alkyl substituted ursolic acid bornyl ester.

[0021] As a further improvement of the present invention, the preparation method of the Chinese medicine polysaccharide is as follows:

[0022] T1. Wash, dry, crush and mix Astragalus, Codonopsis and Platycodon to prepare Chinese medicine powder;

[0023] T2. Add the Chinese medicine powder into water, add cellulase, perform enzymolysis, heat and boil to extract, filter, add ethanol to the filtrate for precipitation, filter, wash, and dry to obtain Chinese medicine polysaccharides.

[0024] As a further improvement of the present invention, the mass ratio of Astragalus, Codonopsis and Platycodon in step T1 is 10-12:3-5:5-7; the solid-liquid ratio of the Chinese medicine powder and water in step T2 is 1:5-7 g / mL, the amount of cellulase added is 3-5wt% of the total mass of the system, the temperature of the enzymatic hydrolysis is 50-60°C, the time is 1-3h, the extraction time is 3-5h, the ethanol is added to 70-75wt% of the ethanol content of the system, and the precipitation time is 2-4h.

[0025] As a further improvement of the present invention, the preparation method of the algae polysaccharide is as follows:

[0026] U1. The Gexian rice algae and rock algae are dried, crushed, and mixed to obtain algae powder;

[0027] U2. Add the algae powder in step U1 to water, heat and boil to extract, filter, retain the solid, and obtain an aqueous solution;

[0028] U3. The solid in step U2 is added to water, a composite enzyme is added, sterilized, inoculated with a seed solution of Bacillus subtilis, cultured by enzymatic fermentation, filtered, and an enzymatic fermentation broth is obtained;

[0029] U4. Mix the aqueous solution in step U2 and the enzymatic fermentation liquid in step U3, add ethanol for precipitation, filter, wash and dry the solid to obtain algae polysaccharide.

[0030] As a further improvement of the present invention, the mass ratio of the algae and the rock algae in step U1 is 3-5:6-8; the solid-liquid ratio of the algae powder and water in step U2 is 1:7-10 g / mL, and the extraction time is 2-4 hours; the composite enzyme in step U3 is cellulase and pectinase, the mass ratio is 7-10:2-4, the mass ratio of the solid, water, and composite enzyme is 10-12:100:2-4, and the bacterial content of the Bacillus subtilis seed liquid is 10 8 -10 9 cfu / mL, the inoculation amount of the Bacillus subtilis seed liquid is 1-2v / v%, the conditions of the enzymatic fermentation culture are 40-45°C, 70-100r / min, and the enzymatic fermentation culture is 24-48h; the mass ratio of the aqueous solution and the enzymatic fermentation liquid in step U4 is 10-12:20-25, the content of ethanol added to the system is 70-75wt%, and the precipitation time is 3-5h.

[0031] The present invention further protects a method for preparing the above skin care composition, comprising the following steps:

[0032] (1) dissolving ectoine and the polysaccharide composition in purified water, stirring and mixing uniformly to obtain an aqueous phase;

[0033] (2) adding glycerol glucoside and the penetration enhancer composition to jojoba oil, stirring and mixing uniformly to prepare an oil phase;

[0034] (3) The water phase and the oil phase are mixed, carbomer is added, emulsified, and filtered to prepare a skin care composition.

[0035] The present invention further protects the use of the above skin care composition in skin moisturizing, whitening and anti-oxidation.

[0036] The present invention has the following beneficial effects:

[0037] Glycerol glucoside is a glycoside compound formed by a molecule of glycerol and a molecule of glucose connected by glycosides. It can lock moisture for cells, improve dry skin, and play a moisturizing effect. It promotes the further processing of filaggrin into amino acids in the upper epidermal stratum corneum, helping the skin to lock moisture, thereby improving the skin barrier, stimulating the proliferation of subcutaneous collagen, and tightening the skin; Ecdoin can soothe the skin, and can also play a sedative role, repair damaged skin, achieve skin regeneration, increase the hydrophilicity of the skin, promote the synthesis of extracellular hyaluronic acid, glycoprotein and other macromolecules, improve the microcirculation of the skin, and play a moisturizing effect. The synergistic effect of the two can increase skin moisture, reduce skin sensitivity, whiten, tighten, and improve skin elasticity, and has a good skin care effect.

[0038] The fusilli algae contains rich polysaccharides, which have good moisturizing, anti-oxidation and skin damage repairing effects, can reduce the activity of tyrosinase in A375 cells, can inhibit the generation of melanin, and have whitening function; the polysaccharides extracted from the fusilli can effectively inhibit the generation of melanin, inhibit the activity of tyrosinic acid by absorbing ultraviolet rays, can effectively inhibit the generation of skin melanin, effectively prevent the appearance of spots, and have good radiation protection effect. The polysaccharide obtained by mixing the polysaccharide obtained by direct water extraction and the enzymatic fermentation polysaccharide obtained by promoting the rupture of the algae cell wall through enzymatic fermentation has good physiological activity and synergistic effect.

[0039] Chinese herbal polysaccharides are active Chinese herbal polysaccharides obtained by extracting materials such as astragalus, codonopsis, and platycodon. These polysaccharides inhibit the expression of chemokines and adhesion factors and the activity of key enzymes in the inflammatory process through combined action, secrete and promote cell proliferation, tissue filling and re-epithelialization, enhance the secretion of hydroxyproline by human fibroblasts, and promote the synthesis of collagen, thereby promoting skin repair and improving skin elasticity. It can also play a good antioxidant role by scavenging free radicals, enhancing the activity of antioxidant enzymes, inhibiting the production of lipid peroxides, protecting organelles, and inhibiting cell apoptosis.

[0040] The present invention further prepares and adds a penetration enhancer composition, including alkyl-substituted ursolic acid bornyl ester and menthol, which work synergistically to significantly promote the transdermal absorption of active components, easily penetrate into the dermis of the skin, and are conducive to being absorbed by the skin, thereby greatly improving the skin care effect. The alkyl-substituted ursolic acid bornyl ester is composed of ursolic acid, borneol and an alkyl chain, and the preparation method is simple and the conditions are mild. The long-chain alkyl therein can disturb the phospholipid bilayer, thereby promoting the active component to enter the dermis cells and exert the effect. At the same time, the irritation of ursolic acid can be reduced, and the toxic and side effects caused by the sublimation of borneol can be avoided. The prepared alkyl-substituted ursolic acid bornyl ester is less irritating and safe, and also has good auxiliary whitening, antibacterial and anti-inflammatory effects.

[0041] The skin care composition prepared by the present invention has a wide source of raw materials, is safe and non-irritating, has a simple preparation method, and has low cost. It has good moisturizing, reduces skin sensitivity, whitens, tightens, improves skin elasticity, has antibacterial and anti-inflammatory effects, and repairs skin, and has broad application prospects. DETAILED DESCRIPTION

[0042] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0043] Cellulase, 10,000 U / g, and pectinase, 10,000 U / g, were purchased from Nanning Dongheng Huadao Biotechnology Co., Ltd.

[0044] The preparation method of Bacillus subtilis (ATCC9372, purchased from Beijing Anjielong Technology Co., Ltd.) seed solution is as follows: Bacillus subtilis is inoculated into Gould's medium, and activated and cultured for 18 hours at 50°C and 100 r / min under aerobic conditions to obtain a culture medium with a bacterial content of 10 8 -10 9 cfu / mL of Bacillus subtilis seed liquid.

[0045] Preparation Example 1 Preparation of Alkyl Substituted Ursolic Acid Bornyl Ester

[0046] Synthesis route:

[0047]

[0048] The specific method is as follows:

[0049] S1. Add 0.115 mol ursolic acid and 0.1 mol borneol to 200 mL toluene, add 4 wt% concentrated sulfuric acid to the total mass of the system, heat to reflux for 7 h, cool to room temperature, filter, wash, and dry to obtain ursolic acid borneol ester; ESI-MS calculated value: C 40 H 65 O3(M+H) + 593.49, found: 593.5, yield: 65%.

[0050] NMR results: 1 H NMR (300MHz, CDCl3) δ5.29 (m, 1H), 3.82 (t, 1H), 3.15 (t, 1H), 2.71 (d, 1H), 2.0 (br, 1H), 1.90 (d, 2H), 1.77 (t, 2H), 1.59-1.65(m, 8H), 1.37-1.42(m, 14H), 1.24-1.27(m, 6H), 1.15-1.18(m, 9H), 1.11(s, 12H), 1.02(d, 6H).

[0051] S2. Add 0.115 mol ursolic acid bornyl ester and 0.4 mol triethylamine to 200 mL acetonitrile, add 0.1 mol 1-chlorododecane, heat to 55°C, stir to react for 2 h, cool to room temperature, filter, wash, and recrystallize from ethyl acetate to obtain alkyl substituted ursolic acid bornyl ester. ESI-MS calculated value: C 52 H 89 O3(M+H) + 761.67, found: 761.7, yield: 88%.

[0052] NMR results: 1 H NMR (300MHz, CDCl3) δ5.27 (m, 1H), 3.84 (t, 1H), 3.37 (t, 2H), 3.17 (t, 1H), 2.72 (d, 1H), 1.90 (d, 2H), 1.77 (t, 2H) , 1.59-1.65(m, 8H), 1.37-1.46(m, 16H), 1.25-1.31(m, 24H), 1.15-1.18(m, 9H), 1.11(s, 12H), 0.97-1.01(d, 9H).

[0053] Preparation Example 2 Preparation of Chinese Medicine Polysaccharide

[0054] Here’s how:

[0055] T1 10 parts by weight of Astragalus, 3 parts by weight of Codonopsis, 5 parts by weight of Platycodon grandiflorum were washed, dried, crushed and mixed to obtain a Chinese medicine powder;

[0056] T2. Add Chinese herbal medicine powder into water, wherein the solid-liquid ratio of the Chinese herbal medicine powder to water is 1:5 g / mL, add cellulase in an amount of 3 wt% of the total mass of the system, perform enzymolysis at 50°C for 1 hour, heat and boil for extraction for 3 hours, filter, add ethanol to the filtrate until the ethanol content of the system is 70 wt%, precipitate for 2 hours, filter, wash, and dry to obtain Chinese herbal medicine polysaccharides.

[0057] Preparation Example 3 Preparation of Chinese medicine polysaccharides

[0058] Here’s how:

[0059] T1 12 parts by weight of Astragalus, 5 parts by weight of Codonopsis, 7 parts by weight of Platycodon grandiflorum were washed, dried, crushed and mixed to obtain a Chinese medicine powder;

[0060] T2. Add Chinese herbal medicine powder into water, wherein the solid-liquid ratio of the Chinese herbal medicine powder to water is 1:7 g / mL, add cellulase in an amount of 5wt% of the total mass of the system, perform enzymolysis at 60°C for 3h, heat and boil for extraction for 5h, filter, add ethanol to the filtrate until the ethanol content of the system is 75wt%, precipitate for 4h, filter, wash, and dry to obtain Chinese herbal medicine polysaccharide.

[0061] Preparation Example 4 Preparation of Chinese Medicine Polysaccharide

[0062] Here’s how:

[0063] T1 11 parts by weight of Astragalus, 4 parts by weight of Codonopsis, 6 parts by weight of Platycodon grandiflorum were washed, dried, crushed and mixed to obtain a Chinese medicine powder;

[0064] T2. Add Chinese herbal medicine powder into water, wherein the solid-liquid ratio of the Chinese herbal medicine powder to water is 1:6 g / mL, add cellulase in an amount of 4 wt% of the total mass of the system, perform enzymolysis at 55°C for 2 h, heat and boil for extraction for 4 h, filter, add ethanol to the filtrate until the ethanol content of the system is 72 wt%, precipitate for 3 h, filter, wash, and dry to obtain Chinese herbal medicine polysaccharides.

[0065] Comparative Preparation Example 1

[0066] The difference compared with Preparation Example 4 is that no cellulase was added.

[0067] Preparation Example 5 Preparation of Algae Polysaccharide

[0068] Here’s how:

[0069] U1. 3 parts by weight of Gexian rice algae and 6 parts by weight of rockweed were dried, crushed and mixed to obtain algae powder;

[0070] U2. Add the algae powder in step U1 to water, wherein the solid-liquid ratio of the algae powder to water is 1:7 g / mL, heat and boil to extract for 2 hours, filter, retain the solid, and obtain an aqueous solution;

[0071] U3. Add 10 parts by weight of the solid in step U2 to 100 parts by weight of water, add 2 parts by weight of the complex enzyme, sterilize, inoculate with Bacillus subtilis seed solution, the inoculation amount is 1v / v%, 40°C, 70r / min, enzymatic fermentation culture for 24h, filter, and obtain enzymatic fermentation broth;

[0072] The complex enzyme is cellulase and pectinase, with a mass ratio of 7:2;

[0073] U4. Mix 10 parts by weight of the aqueous solution in step U2 and 20 parts by weight of the enzymatic fermentation liquid in step U3, add ethanol until the ethanol content in the system is 70wt%, precipitate for 3 hours, filter, wash and dry the solid to obtain algae polysaccharide.

[0074] Preparation Example 6 Preparation of Algae Polysaccharide

[0075] Here’s how:

[0076] U1 5 parts by weight of Gexian rice algae and 8 parts by weight of rock algae were dried, crushed and mixed to obtain algae powder;

[0077] U2. Add the algae powder in step U1 to water, wherein the solid-liquid ratio of the algae powder to water is 1:10 g / mL, heat and boil to extract for 4 hours, filter, retain the solid, and obtain an aqueous solution;

[0078] U3. Add 12 parts by weight of the solid in step U2 to 100 parts by weight of water, add 4 parts by weight of the complex enzyme, sterilize, inoculate with Bacillus subtilis seed solution, the inoculation amount is 2v / v%, 45°C, 100r / min, enzymatic fermentation culture for 48h, filter, and obtain enzymatic fermentation broth;

[0079] The complex enzyme is cellulase and pectinase, with a mass ratio of 10:4;

[0080] U4. Mix 12 parts by weight of the aqueous solution in step U2 and 25 parts by weight of the enzymatic fermentation liquid in step U3, add ethanol until the ethanol content in the system is 75wt%, precipitate for 5 hours, filter, wash and dry the solid to obtain algae polysaccharide.

[0081] Preparation Example 7 Preparation of Algae Polysaccharide

[0082] Here’s how:

[0083] U1. 4 parts by weight of Gexian rice algae and 7 parts by weight of rockweed were dried, crushed and mixed to obtain algae powder;

[0084] U2. Add the algae powder in step U1 to water, wherein the solid-liquid ratio of the algae powder to water is 1:8 g / mL, heat and boil to extract for 3 hours, filter, retain the solid, and obtain an aqueous solution;

[0085] U3. Add 11 parts by weight of the solid in step U2 to 100 parts by weight of water, add 3 parts by weight of the complex enzyme, sterilize, inoculate with Bacillus subtilis seed solution, the inoculation amount is 1.4v / v%, 42°C, 85r / min, enzymatic fermentation culture for 36h, filter, and obtain enzymatic fermentation broth;

[0086] The complex enzyme is cellulase and pectinase, with a mass ratio of 8:3;

[0087] U4. Mix 11 parts by weight of the aqueous solution in step U2 and 22 parts by weight of the enzymatic fermentation liquid in step U3, add ethanol until the ethanol content in the system is 72wt%, precipitate for 4 hours, filter, wash and dry the solid to obtain algae polysaccharide.

[0088] Preparation Example 8

[0089] Compared with Preparation Example 7, the difference is that the complex enzyme is a single cellulase.

[0090] Preparation Example 9

[0091] Compared with Preparation Example 7, the difference is that the complex enzyme is a single pectinase.

[0092] Comparative Preparation Example 2

[0093] Compared with Preparation Example 7, the difference is that no complex enzyme is added.

[0094] Comparative Preparation Example 3

[0095] Compared with Preparation Example 7, the difference is that the Bacillus subtilis seed liquid is not inoculated.

[0096] Comparative Preparation Example 4

[0097] Compared with Preparation Example 7, the difference is that no Myriophyllum puerariae was added.

[0098] Comparative Preparation Example 5

[0099] The difference compared with Preparation Example 7 is that no fucoidan was added.

[0100] Example 1

[0101] This embodiment provides a method for preparing a skin care composition, comprising the following steps:

[0102] (1) mixing the alkyl-substituted ursolic acid bornyl ester and menthol prepared in Preparation Example 1 in a mass ratio of 12:2 to prepare a penetration enhancer composition;

[0103] (2) The traditional Chinese medicine polysaccharide prepared in Preparation Example 2, the algae polysaccharide prepared in Preparation Example 5, and hyaluronic acid were mixed in a mass ratio of 7:3:1 to prepare a polysaccharide composition;

[0104] (3) dissolving 1 part by weight of ectoine and 12 parts by weight of the polysaccharide composition in 20 parts by weight of purified water, stirring and mixing for 15 minutes to prepare an aqueous phase;

[0105] (4) adding 3 parts by weight of glycerol glucoside and 0.1 parts by weight of the penetration enhancer composition to 10 parts by weight of jojoba oil, stirring and mixing for 15 minutes to prepare an oil phase;

[0106] (5) The aqueous phase and the oil phase were mixed, 0.3 parts by weight of carbomer was added, emulsified at 7000 r / min for 15 min, and filtered to prepare a skin care composition.

[0107] Example 2

[0108] This embodiment provides a method for preparing a skin care composition, comprising the following steps:

[0109] (1) mixing the alkyl-substituted ursolic acid bornyl ester prepared in Preparation Example 1 and menthol in a mass ratio of 15:4 to prepare a penetration enhancer composition;

[0110] (2) The traditional Chinese medicine polysaccharide prepared in Preparation Example 3, the algae polysaccharide prepared in Preparation Example 6, and hyaluronic acid were mixed in a mass ratio of 10:5:2 to prepare a polysaccharide composition;

[0111] (3) dissolving 2 parts by weight of ectoine and 15 parts by weight of the polysaccharide composition in 40 parts by weight of purified water, stirring and mixing for 15 minutes to prepare an aqueous phase;

[0112] (4) adding 5 parts by weight of glyceryl glucoside and 0.2 parts by weight of the penetration enhancer composition to 15 parts by weight of jojoba oil, stirring and mixing for 15 minutes to prepare an oil phase;

[0113] (5) The aqueous phase and the oil phase were mixed, 0.5 parts by weight of carbomer was added, emulsified at 7000 r / min for 15 min, and filtered to prepare a skin care composition.

[0114] Example 3

[0115] This embodiment provides a method for preparing a skin care composition, comprising the following steps:

[0116] (1) mixing the alkyl-substituted ursolic acid bornyl ester and menthol prepared in Preparation Example 1 in a mass ratio of 13:3 to prepare a penetration enhancer composition;

[0117] (2) The traditional Chinese medicine polysaccharide prepared in Preparation Example 3, the algae polysaccharide prepared in Preparation Example 7, and hyaluronic acid were mixed in a mass ratio of 8:4:1.5 to prepare a polysaccharide composition;

[0118] (3) dissolving 1.5 parts by weight of ectoine and 13 parts by weight of the polysaccharide composition in 30 parts by weight of purified water, stirring and mixing for 15 minutes to prepare an aqueous phase;

[0119] (4) adding 4 parts by weight of glycerol glucoside and 0.15 parts by weight of the penetration enhancer composition to 12 parts by weight of jojoba oil, stirring and mixing for 15 minutes to prepare an oil phase;

[0120] (5) The aqueous phase and the oil phase were mixed, 0.4 parts by weight of carbomer was added, emulsified at 7000 r / min for 15 min, and filtered to prepare a skin care composition.

[0121] Embodiment 4-5

[0122] Compared with Example 3, the difference is that the algae polysaccharide is prepared by Preparation Examples 8 and 9 respectively.

[0123] Comparative Example 1

[0124] Compared with Example 3, the difference is that the Chinese medicine polysaccharide is prepared by Comparative Preparation Example 1.

[0125] Comparative Examples 2-5

[0126] Compared with Example 3, the difference is that the algae polysaccharide is prepared by comparative preparation examples 2-5 respectively.

[0127] Comparative Example 6

[0128] Compared with Example 3, the difference is that the penetration enhancer composition is a single alkyl-substituted ursolic acid bornyl ester.

[0129] Comparative Example 7

[0130] Compared with Example 3, the difference is that the penetration enhancer composition is a single menthol.

[0131] Comparative Example 8

[0132] Compared with Example 3, the difference is that no penetration enhancer composition is added.

[0133] Comparative Example 9

[0134] Compared with Example 3, the difference is that no algae polysaccharide is added.

[0135] Comparative Example 10

[0136] Compared with Example 3, the difference is that no Chinese medicine polysaccharide is added.

[0137] Comparative Example 11

[0138] Compared with Example 3, the difference is that no ectoine is added.

[0139] Comparative Example 12

[0140] The difference compared with Example 3 is that glycerol glucoside is not added.

[0141] Comparative Example 13

[0142] Compared with Example 3, the difference is that ectoine and glycerol glucoside are not added.

[0143] Test Example 1 Antioxidant Activity Test

[0144] The skin care compositions prepared in Examples 1-5 and Comparative Examples 1-13 were diluted 1000 times with water to prepare sample solutions. The results are shown in Table 1.

[0145] 1. DPPH free radical scavenging rate test method:

[0146] Take 1mL of 2mmol / L DPPH (1,1-diphenyl-2-trinitrophenylhydrazine) working solution and place it in a test tube. Add 1mL of sample solution to the sample group (results are represented by A1); the blank group (results are represented by A2) uses purified water instead of DPPH working solution; the negative control group (results are represented by A3) uses purified water instead of working solution; the positive control group uses vitamin C (concentration of 0.01wt‰) instead of sample solution. Mix all reagents evenly, and after 30 minutes of light protection, repeat the test 3 times, use an ultraviolet spectrophotometer to measure the absorbance value at 517nm, and take the average value to calculate the scavenging rate. The calculation formula for DPPH free radical scavenging rate is:

[0147] DPPH free radical scavenging rate (%) = [1-(A2-A1) / A3] × 100%

[0148] 2. ABTS + Free radical scavenging rate determination method

[0149] 0.2 mL ABTS + The working solution of (2,2-azino-bis(3-ethyl-benzothiazole-6-sulfonic acid)) (absorbance at 734 nm was 0.70±0.02) was transferred to the detection well of the antioxidant kit, and the sample detection well (results were measured by A i 10 μL of sample solution was added to each well; the blank well (the result is indicated by A0) was replaced with purified water instead of sample solution; the control well (the result is indicated by A j Phosphate buffer solution (pH 6.7) (used to prepare ABTS + Working fluid) instead of ABTS +Working solution. The positive control group used vitamin C (concentration of 0.01wt%) instead of the sample solution. After mixing, place the kit at room temperature and away from light for 8 minutes, and use an ultraviolet spectrophotometer to measure its absorbance at a wavelength of 734nm. Repeat the operation 3 times and calculate the clearance rate. The clearance rate is calculated as follows:

[0150] ABTS + Base clearance rate (%) = [1-(A i -A j ) / A0]×100%

[0151] Table 1

[0152]

[0153]

[0154] It can be seen from the above table that the skin care compositions prepared in Examples 1-3 of the present invention have good antioxidant effects.

[0155] Test Example 2 Tyrosinase Activity Assay

[0156] The skin care compositions prepared in Examples 1-5 and Comparative Examples 1-13 were diluted 1000 times with water to prepare sample solutions. According to Table 2, phosphate buffer solution with pH=6.8, sample solution and tyrosinase solution were added to the test tube in sequence and mixed thoroughly. After 10 minutes in a 37°C water bath, 1 mL of 0.45 mg / mL L-tyrosine solution was added and mixed evenly, and the timing was started immediately. After the system reacted for 10 minutes, the absorbance value at 475 nm was measured with phosphate buffer solution with pH=6.8 as a blank control. The total reaction system was 5 mL. The results are shown in Table 3.

[0157] The inhibition rate of tyrosinase was calculated according to the following formula:

[0158] Tyrosinase inhibition rate (%) = [(A1-A2)-(A3-A4)] / (A1-A2)×100%

[0159] Among them: A1 does not contain sample solution but contains tyrosinase; A2 does not contain sample solution and does not contain tyrosinase; A3 contains sample solution and tyrosinase; A4 contains sample solution but does not contain tyrosinase.

[0160] Table 2

[0161]

[0162] Table 3

[0163] Group Tyrosinase inhibition rate (%) Example 1 89.46 Example 2 90.01 Example 3 91.58 Example 4 87.09 Example 5 86.94 Comparative Example 1 86.79 Comparative Example 2 85.32 Comparative Example 3 84.19 Comparative Example 4 84.72 Comparative Example 5 83.11 Comparative Example 6 81.29 Comparative Example 7 84.55 Comparative Example 8 79.73 Comparative Example 9 82.24 Comparative Example 10 84.18 Comparative Example 11 83.09 Comparative Example 12 85.67 Comparative Example 13 78.98

[0164] It can be seen from the above table that the skin care compositions prepared in Examples 1-3 of the present invention have good tyrosinase inhibitory activity and good whitening effect.

[0165] Test Example 3 Human skin patch test and allergy test

[0166] Test samples: skin care compositions prepared in Examples 1-5 and Comparative Examples 1-13 of the present invention.

[0167] Experimental method: Subjects aged 18-54 were selected and randomly divided into 18 groups, with 6 people in each group. Among them, the subject's right forearm flexor side was marked with a 5cm×5cm area and medical disinfection was used to create an injury in the marked area. The method was: 36-needle microneedle introduced nutrient solution for 30s, and a cotton ball soaked in physiological saline was used to gently wipe the residual liquid to keep the marked area dry; the test samples were placed in the 1-18 spot tester wells, respectively, with a dosage of 10-20μL. Bathing was prohibited during the test, and the normal reaction was negative. The test samples were applied to the face, neck and back of the ear of the subject, and the skin condition of the subject was observed after 10 minutes. The results are shown in Table 4.

[0168] Table 4

[0169] Group Patch reaction Facial skin Neck skin Skin behind the ear Example 1 Negative No allergy No allergy No allergy Example 2 Negative No allergy No allergy No allergy Example 3 Negative No allergy No allergy No allergy Example 4 Negative No allergy No allergy No allergy Example 5 Negative No allergy No allergy No allergy Comparative Example 1 Negative No allergy No allergy No allergy Comparative Example 2 Negative No allergy No allergy No allergy Comparative Example 3 Negative No allergy No allergy No allergy Comparative Example 4 Negative No allergy No allergy No allergy Comparative Example 5 Negative No allergy No allergy No allergy Comparative Example 6 Negative No allergy No allergy No allergy Comparative Example 7 Negative No allergy No allergy No allergy Comparative Example 8 Negative No allergy No allergy No allergy Comparative Example 9 Negative No allergy No allergy No allergy Comparative Example 10 Negative No allergy No allergy No allergy Comparative Example 11 Negative No allergy No allergy No allergy Comparative Example 12 Negative No allergy No allergy No allergy Comparative Example 13 Negative No allergy No allergy No allergy

[0170] As can be seen from the above table, the patch reactions of the skin care compositions prepared in Examples 1-5 and Comparative Examples 1-13 of the present invention are negative reactions, and they are safe to use without any allergic reactions.

[0171] Test Example 4 Experiment on promoting the synthesis of type III collagen

[0172] The skin care compositions prepared in Examples 1-5 and Comparative Examples 1-13 were diluted 1000 times with water to prepare sample solutions. Human fibroblasts (purchased from Merck Life Science Co., Ltd.) cultured in DMEM (dulbecco's modified eagle medium) containing 12% FBS (fetal bovine serum) were inoculated in a 96-well plate. After the cells attached, the medium was exchanged with DMEM containing 0.2wt% FBS (fetal bovine serum) and 250μmol / L magnesium ascorbyl phosphate, and 100μL of sample solution (100μL of deionized water was added to the control group) was added respectively, mixed evenly, and after culturing for 72h, the supernatant was collected and centrifuged. The content of type III collagen in the obtained supernatant was determined using a kit, and the synthesis promotion rate of type III collagen was calculated. The results are shown in Table 5.

[0173] Type III collagen synthesis promotion rate (%) = (A1-A0) / A0×100%

[0174] A1: the amount of type III collagen produced after adding the sample;

[0175] A0: The amount of type III collagen produced by the sample without addition.

[0176] Table 5

[0177] Group Type III collagen synthesis promotion rate (%) Example 1 274 Example 2 277 Example 3 282 Example 4 259 Example 5 255 Comparative Example 1 266 Comparative Example 2 249 Comparative Example 3 242 Comparative Example 4 245 Comparative Example 5 239 Comparative Example 6 227 Comparative Example 7 249 Comparative Example 8 215 Comparative Example 9 227 Comparative Example 10 252 Comparative Example 11 220 Comparative Example 12 235 Comparative Example 13 207

[0178] It can be seen from the above table that the skin care compositions prepared in Examples 1-3 of the present invention have a good effect of promoting collagen production.

[0179] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A skin care composition, characterized in that The method is prepared from the following raw materials in parts by weight: 3-5 parts of glycerol glucoside, 1-2 parts of ectoine, 12-15 parts of a polysaccharide composition, 0.1-0.2 parts of a penetration enhancer composition, 0.3-0.5 parts of carbomer, 10-15 parts of jojoba oil, and 20-40 parts of purified water; The penetration enhancer composition is composed of alkyl-substituted ursolic acid bornyl and menthol, with a mass ratio of 12-15:2-4; The structural formula of the alkyl-substituted ursolic acid bornyl ester is shown in Formula I: Wherein, R = C6-C12 alkyl chain; The polysaccharide composition is composed of traditional Chinese medicine polysaccharides, algae polysaccharides, and hyaluronic acid, with a mass ratio of 7-10:3-5:1-2; The preparation method of the Chinese medicine polysaccharide is as follows: T1. Wash, dry, crush and mix Astragalus, Codonopsis and Platycodon grandiflorum to prepare Chinese medicine powder; T2. Add the Chinese medicine powder to water, add cellulase, perform enzymolysis, heat and boil to extract, filter, add ethanol to the filtrate for precipitation, filter, wash, and dry to obtain Chinese medicine polysaccharide; The preparation method of the algae polysaccharide is as follows: U1. The Gexian rice algae and rock algae are dried, crushed, and mixed to obtain algae powder; U2. Add the algae powder in step U1 to water, heat and boil to extract, filter, retain the solid, and obtain an aqueous solution; U3. Add the solid in step U2 to water, add a composite enzyme, sterilize, inoculate Bacillus subtilis seed solution, culture by enzymatic fermentation, filter, and obtain an enzymatic fermentation broth; the composite enzyme is cellulase and pectinase, and the mass ratio is 7-10:2-4; U4. Mix the aqueous solution in step U2 and the enzymatic fermentation liquid in step U3, add ethanol for precipitation, filter, wash and dry the solid to obtain algae polysaccharide.

2. The skin care composition according to claim 1, characterized in that The preparation method of the alkyl-substituted ursolic acid bornyl ester is as follows: S1. reacting ursolic acid and borneol to obtain ursolic acid borneol ester; S2. reacting ursolic acid bornyl ester with an alkyl halide to obtain an alkyl-substituted ursolic acid bornyl ester.

3. The skin care composition according to claim 2, characterized in that: The molar ratio of ursolic acid to borneol in step S1 is 1.1-1.2:1, the reaction temperature is 100-120°C, and the reaction time is 6-8h; the molar ratio of ursolic acid borneol ester to alkyl halide in step S2 is 1.1-1.2:1, the reaction temperature is 50-60°C, and the reaction time is 1-3h, and the alkyl halide is selected from at least one of 1-chlorohexane, 1-bromohexane, 1-chloroheptane, 1-bromoheptane, 1-chlorooctane, 1-bromooctane, 1-chlorononane, 1-bromononane, 1-chlorodecane, 1-bromodecane, 1-chloroundecane, 1-bromodecane, 1-chlorododecane, and 1-bromododecane.

4. The skin care composition according to claim 2, characterized in that: The preparation method of the alkyl-substituted ursolic acid bornyl ester is as follows: S1. Add 1.1-1.2 molar equivalents of ursolic acid and 1 molar equivalent of borneol to toluene, add 3-5wt% of concentrated sulfuric acid to the total mass of the system, heat to reflux for 6-8h, cool to room temperature, filter, wash, and dry to obtain ursolic acid borneol ester; S2. Add 1.1-1.2 molar equivalents of ursolic acid bornyl ester and 3-5 molar equivalents of triethylamine to acetonitrile, add 1 molar equivalent of alkyl halide, heat to 50-60°C, stir to react for 1-3h, cool to room temperature, filter, wash, and recrystallize from ethyl acetate to obtain alkyl substituted ursolic acid bornyl ester.

5. The skin care composition according to claim 1, characterized in that: The mass ratio of astragalus, codonopsis and platycodon in step T1 is 10-12:3-5:5-7; the solid-liquid ratio of the Chinese medicine powder and water in step T2 is 1:5-7 g / mL, the amount of cellulase added is 3-5wt% of the total mass of the system, the temperature of the enzymolysis is 50-60°C, the time is 1-3h, the extraction time is 3-5h, the ethanol is added to 70-75wt% of the ethanol content of the system, and the precipitation time is 2-4h.

6. The skin care composition according to claim 1, characterized in that: The mass ratio of Gexianmi Algae and Rock Algae in step U1 is 3-5:6-8; the solid-liquid ratio of algae powder and water in step U2 is 1:7-10 g / mL, and the extraction time is 2-4 h; the mass ratio of solid, water, and complex enzyme in step U3 is 10-12:100:2-4, and the bacterial content of the Bacillus subtilis seed liquid is 10 8 -10 9 cfu / mL, the inoculation amount of the Bacillus subtilis seed liquid is 1-2v / v%, the conditions of the enzymatic fermentation culture are 40-45°C, 70-100r / min, and the enzymatic fermentation culture is 24-48h; the mass ratio of the aqueous solution and the enzymatic fermentation liquid in step U4 is 10-12:20-25, the content of ethanol added to the system is 70-75wt%, and the precipitation time is 3-5h.

7. A method for preparing the skin care composition according to any one of claims 1 to 6, characterized in that: The following steps are involved: (1) dissolving ectoine and the polysaccharide composition in purified water, stirring and mixing uniformly to obtain an aqueous phase; (2) adding glycerol glucoside and the penetration enhancer composition to jojoba oil, stirring and mixing uniformly to prepare an oil phase; (3) The water phase and the oil phase are mixed, carbomer is added, emulsified, and filtered to prepare a skin care composition.

8. Use of the skin care composition according to any one of claims 1 to 7 in the preparation of skin moisturizing, whitening and anti-oxidation cosmetics.

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