Anti-aging cosmetics and preparation method and application thereof

Abstract

The present invention proposes an anti-aging cosmetic and its preparation method and application, belonging to the field of cosmetic technology. Prepared by the following raw materials by weight: 3-5 parts of β-nicotinamide mononucleotide, 1-2 parts of ergothioneine, 0.1-0.2 parts of permeation enhancer composition, 0.3-0.5 parts of carbomer, 1-2 parts of composite peptide composition, 3-5 parts of grape seed oil and 15-20 parts of purified water. The anti-aging cosmetics prepared by the present invention have a wide source of raw materials, are safe and non-irritating, have a simple preparation method, are relatively low in cost, have good whitening, anti-allergy, anti-inflammatory, improve skin elasticity, improve skin condition, delay aging and other effects, and have broad application prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and in particular to an anti-aging cosmetic and a preparation method and application thereof. Background Art

[0002] The skin is the largest organ covering the human body. It is very susceptible to damage due to direct contact with the external environment and the stimulation of various stress factors such as oxidation, dryness and ultraviolet rays. At the same time, due to the influence of internal factors such as age, diet and living habits, the skin function declines and genetic abnormalities make the skin more susceptible to aging. Since the skin is on the outermost side of the human body, it clearly shows the beauty of the human body. Therefore, anti-aging cosmetics have become one of the products urgently needed by the majority of female consumers.

[0003] Anti-aging cosmetics have accounted for more than 50% of the cosmetics market. One of the most important factors of skin aging is skin photoaging caused by long-term exposure to ultraviolet radiation. Skin photoaging is caused by the increase of free radicals in the skin. Free radicals can damage biological membranes, promote the increase and amorphization of elastin fibers, and significantly reduce collagen fibers and increase glycosaminoglycans. Fighting and eliminating free radicals to prevent free radical damage is often achieved through antioxidants.

[0004] At present, antioxidants are divided into two categories: one is enzyme antioxidants, among which superoxide dismutase is the most widely used. However, this type of antioxidant has poor stability in cosmetics, and its molecular weight is large and cannot be absorbed, so its use is limited; the other type is vitamin series non-enzyme antioxidants, such as vitamin A, vitamin E, vitamin C, coenzyme Q10, etc., but this type of antioxidant also has poor stability, easy to change color and cause skin allergies, so their use is also subject to some restrictions. There are very few skin care products on the market that have few side effects, are safe and stable, have excellent antioxidant effects, and have comprehensive and long-lasting anti-aging effects. Summary of the invention

[0005] The purpose of the present invention is to provide an anti-aging cosmetic and its preparation method and application. The raw material source is wide, safe and non-irritating, the preparation method is simple, the cost is low, and it has good whitening, anti-allergic, anti-inflammatory, skin elasticity improvement, skin condition improvement, anti-aging and other effects, and has broad application prospects.

[0006] The technical solution of the present invention is achieved in this way:

[0007] The present invention provides an anti-aging cosmetic, which is prepared from the following raw materials by weight: 3-5 parts of β-nicotinamide mononucleotide, 1-2 parts of ergothioneine, 0.1-0.2 parts of a penetration enhancer composition, 0.3-0.5 parts of carbomer, 1-2 parts of a composite peptide composition, 3-5 parts of grape seed oil and 15-20 parts of purified water;

[0008] The penetration enhancer composition is composed of a novel penetration enhancer and a small molecule alcohol in a mass ratio of 5-7:1-2. The structural formula of the novel penetration enhancer is shown in Formula I:

[0009]

[0010] Wherein, R = C6-C12 alkyl chain;

[0011] The composite peptide composition consists of algae protein peptide, blue copper peptide and acetyl tetrapeptide, and the mass ratio is 15-20:3-5:1-2.

[0012] As a further improvement of the present invention, the small molecule alcohol is selected from at least one of glycerol, propylene glycol, butylene glycol and ethanol.

[0013] As a further improvement of the present invention, the preparation method of the novel penetration enhancer is as follows:

[0014] S1. reacting menthol and salicylic acid to obtain menthol salicylate;

[0015] S2. Menthol salicylate and dihaloalkane are reacted to obtain an intermediate having the following structure:

[0016] S3. reacting the intermediate with caprolactam to obtain a product.

[0017] As a further improvement of the present invention, the molar ratio of menthol to salicylic acid in step S1 is 1:1-1.15; the molar ratio of menthol salicylate to dihaloalkane in step S2 is 1.1-1.2:1, the reaction temperature is 50-60°C, the reaction time is 2-4h, and the dihaloalkane is selected from 1,6-dichlorohexane, 1,6-dibromohexane, 1,7-dichloroheptane, 1,7-dibromoheptane, 1,8-dichlorooctane, At least one of 1,8-dibromooctane, 1,9-dichlorononane, 1,9-dibromononane, 1,10-dichlorodecane, 1,10-dibromodecane, 1,11-dichloroundecane, 1,11-dibromodecane, 1,12-dichlorododecane and 1,12-dibromodecane; the molar ratio of the intermediate to caprolactam in step S3 is 1:1.1-1.2, the reaction temperature is 75-85°C, and the reaction time is 1-2h.

[0018] As a further improvement of the present invention, the preparation method of the novel penetration enhancer is specifically as follows:

[0019] S1. Add 1 molar equivalent of menthol and 1-1.15 molar equivalent of salicylic acid to toluene, add 2-4wt% concentrated sulfuric acid based on the total mass of the system, heat to reflux, stir to react for 5-7h, cool to room temperature, filter, wash, and dry to obtain menthol salicylate;

[0020] S2. 1.1-1.2 molar equivalents of menthol salicylate and 3-5 molar equivalents of triethylamine are added to acetonitrile, 1 molar equivalent of dihaloalkane is added, heated to 50-60°C, stirred for 2-4h, cooled to room temperature, filtered, washed, and recrystallized from ethyl acetate to obtain an intermediate;

[0021] S3. Add 1 molar equivalent of the intermediate and 3-5 molar equivalents of potassium carbonate to dimethyl sulfoxide, add 1.1-1.2 molar equivalents of caprolactam, heat to 75-85°C, stir to react for 1-2h, cool to room temperature, filter, and recrystallize from toluene to obtain the product.

[0022] As a further improvement of the present invention, the preparation method of the algae protein peptide is as follows:

[0023] T1. The Spirulina and Chlorella pyrenoidosa were dried, crushed, and mixed to obtain algae powder;

[0024] T2. Add the algae powder obtained in step T1 to water, extract by ultrasonic heating, filter, retain the solid, and freeze-dry the filtrate to obtain algae pigment protein;

[0025] T3. The solid in step T2 is added to water, a composite enzyme is added, the seed solution of Lactobacillus reuteri is inoculated, enzymatic fermentation is performed, filtration is performed, the filtrate is dialyzed, and the permeate is freeze-dried to obtain a small molecule algae protein peptide;

[0026] T4. Evenly mix the phycocyanin protein obtained in step T2 and the small molecule phycocyanin peptide obtained in step T3 to obtain phycocyanin peptide.

[0027] As a further improvement of the present invention, the mass ratio of Spirulina and Chlorella vulgaris in step T1 is 5-7:2-4; the ultrasonic power in the ultrasonic heating extraction in step T2 is 1200-1500W, the heating temperature is 40-50°C, the time is 2-4h, and the solid-liquid ratio of the algae powder and water is 1:5-7g / mL; the mass ratio of the solid, water, and complex enzyme in step T3 is 10-12:100:1-2, the complex enzyme includes cellulase and papain, the mass ratio is 7-10:2-4, the inoculation amount of the Lactobacillus reuteri seed liquid is 2-4v / v%, and the bacterial content of the Lactobacillus reuteri seed liquid is 10 7 -10 8cfu / mL, the conditions of the enzymatic fermentation are under anoxic conditions, 35-40°C, 100-120r / min, the enzymatic fermentation culture is 24-36h, the dialysis bag pore size used in the dialysis is 5k-7kDa, and the dialysis time is 2-4h; the mass ratio of the algae pigment protein and the small molecule algae protein peptide in step T4 is 10-12:7-10.

[0028] As a further improvement of the present invention, the preparation method of the algae protein peptide is as follows:

[0029] T1 5-7 parts by weight of Spirulina, 2-4 parts by weight of Chlorella pyrenoidosa were dried, crushed, and mixed to obtain algae powder;

[0030] T2. The algae powder prepared in step T1 is added to water, wherein the solid-liquid ratio of the algae powder to water is 1:5-7 g / mL, and ultrasonically heated to 40-50°C with a power of 1200-1500 W, extracted for 2-4 hours, filtered, the solid is retained, and the filtrate is freeze-dried to obtain algae pigment protein;

[0031] T3. Add 100 parts by weight of the solid in step T2 into water, add 1-2 parts by weight of the complex enzyme, and inoculate the bacterial content to 10 7 -10 8 cfu / mL of Lactobacillus reuteri seed solution, inoculation amount of 2-4v / v%, under anoxic conditions, 35-40°C, 100-120r / min, enzymatic fermentation culture for 24-36h, filtration, filtration of the filtrate with a dialysis bag with a pore size of 5k-7kDa for 2-4h, freeze-drying the permeate to obtain small molecule algae protein peptides;

[0032] The complex enzyme comprises cellulase and papain in a mass ratio of 7-10:2-4;

[0033] T4. 10-12 parts by weight of the phycocyanin protein prepared in step T2 and 7-10 parts by weight of the small molecule phycocyanin peptide prepared in step T3 are mixed evenly to prepare phycocyanin peptide.

[0034] The present invention further protects a method for preparing the above anti-aging cosmetics, comprising the following steps:

[0035] (1) dissolving β-nicotinamide mononucleotide, ergothioneine, and the composite peptide composition in purified water, stirring and mixing to obtain an aqueous phase;

[0036] (2) adding the penetration enhancer composition to the grape seed oil, stirring and mixing uniformly to obtain an oil phase;

[0037] (3) The water phase and the oil phase are mixed, carbomer is added, emulsified, and filtered to prepare anti-aging cosmetics.

[0038] The present invention further protects the use of the above anti-aging cosmetics in promoting skin repair, anti-aging, anti-allergy and improving skin elasticity.

[0039] The present invention has the following beneficial effects:

[0040] β-Nicotinamide mononucleotide is a naturally occurring biologically active nucleotide and a precursor of NAD+. It has the effects of delaying, improving, and preventing aging. It delays skin aging by participating in a variety of enzymatic processes, including glycolysis, TCA cycle, oxidative phosphorylation, DNA repair, and protein deacetylation. Ergothioneine is a natural antioxidant that can protect cells in the human body. It is safe and non-toxic, reduces the formation of reactive oxygen species, protects cells from radiation damage, improves skin condition, and has a moisturizing effect. Under the synergistic effect of β-Nicotinamide mononucleotide and ergothioneine, it can also participate in enzymatic reactions, reduce reactive oxygen damage, significantly improve skin cell vitality, and play an anti-aging and antioxidant role for the skin.

[0041] The composite peptide composition of the present invention includes algae protein peptide, blue copper peptide and acetyl tetrapeptide, wherein the algae protein peptide is composed of algae pigment protein obtained by direct water extraction of spirulina and protein core chlorella and small molecule algae protein peptide prepared by enzymolysis, fermentation and dialysis, and the algae pigment protein has skin anti-allergy, anti-inflammatory, whitening and other effects, and the small molecule algae protein peptide has good water solubility, high biological activity, good anti-oxidation, and promotes skin elasticity and other effects, and the prepared algae protein has a good anti-aging skin care effect; the blue copper peptide has a small molecular structure, is easily absorbed by the skin, can promote the synthesis of skin matrix, enhance the regeneration ability of skin cell tissue, enable the skin to heal quickly when damaged, and improve the gloss and moisturizing feeling of the skin. Acetyl tetrapeptide can accelerate the metabolism of the skin, promote the generation of collagen, increase the elasticity of the skin, and delay aging. Therefore, the composite peptide composition of the present invention has good whitening, anti-allergy, anti-inflammatory, improve skin elasticity, anti-aging and other effects.

[0042] The present invention also prepares and adds a penetration enhancer composition, including a novel penetration enhancer and a small molecule alcohol, wherein the small molecule alcohol can improve the transdermal absorption effect of the active component on the one hand, and play a synergistic role with the novel penetration enhancer, and can also improve the solubility of the novel penetration enhancer and grape seed oil on the other hand, and the grape seed oil plays a better antioxidant effect. The novel penetration enhancer prepared by the present invention is formed by connecting salicylic acid molecules, menthol molecules and caprolactam molecules, which not only reduces the irritation of salicylic acid, but also increases the boiling point of menthol, avoiding its volatilization and reducing effect. At the same time, the preparation method of the prepared novel penetration enhancer is simple, the conditions are mild, and the prepared product has a good transdermal absorption promoting effect, promotes the active component to enter the dermis, and is absorbed by the underlying cells, and plays a better anti-aging skin care effect.

[0043] The anti-aging cosmetics prepared by the present invention have a wide source of raw materials, are safe and non-irritating, have a simple preparation method, and are of low cost. They have good whitening, anti-allergy, anti-inflammatory, skin elasticity enhancement, skin condition improvement, anti-aging and other effects, and have broad application prospects. DETAILED DESCRIPTION

[0044] 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.

[0045] Cellulase, 10,000 U / g, and papain, 60,000 U / g, were purchased from Nanning Dongheng Huadao Biotechnology Co., Ltd.

[0046] The bacterial content of Lactobacillus reuteri (ATCC23272, purchased from Shanghai Fuxiang Biotechnology Co., Ltd.) was 10 7 -10 8 cfu / mL; the preparation method is as follows: Lactobacillus reuteri is inoculated into a slant culture medium, and activated and cultured for 24 hours at 35°C and 100r / min under anaerobic conditions to obtain a bacterial seed solution.

[0047] Preparation Example 1 Preparation of a new penetration enhancer

[0048] Synthesis route:

[0049]

[0050] The specific method is as follows:

[0051] S1. Add 0.1 mol menthol and 0.112 mol salicylic acid into 200 mL toluene, add 3 wt% concentrated sulfuric acid of the total mass of the system, heat to reflux, stir and react for 6 h, cool to room temperature, filter, wash, and dry to obtain menthol salicylate; ESI-MS calculated value: C 17 H 25 O 3 (M+H) + 277.17, found: 277.2, yield: 74%.

[0052] NMR results: 1 H NMR (300 MHz, CDCl 3)δ7.82 (d, J=6.5Hz, 1H), 7.24 (m, 1H), 6.91 (m, 1H), 6.80 (d, J=5.8Hz, 1H), 5.0 (br, 1H), 3.82 (m, 1H), 2.04(m, 1H), 1.79-1.82(m, 3H), 1.57(m, 1H), 1.39-1.41(m, 4H), 1.02(d, 3H), 0.97(d, 6H).

[0053] S2. Add 0.115 mol of menthol salicylate and 0.4 mol of triethylamine to 200 mL of acetonitrile, add 0.1 mol of 1,6-dichlorohexane, heat to 55°C, stir to react for 3 h, cool to room temperature, filter, wash, and recrystallize from ethyl acetate to obtain an intermediate; ESI-MS calculated value: C 23 H 36 C1O 3 (M+H) + 395.23, found: 395.2, yield: 91%.

[0054] NMR results: 1 H NMR (300 MHz, CDCl 3 )δ7.92(d, J=6.7Hz, 1H), 7.39(m, 1H), 6.88-6.91(m, 2H), 3.90-3.92(m, 3H), 3.35(t, 2H), 2.05(m, 1H), 1.80 (m, 3H), 1.74 (m, 2H), 1.57-1.60 (m, 3H), 1.41-1.44 (m, 4H), 1.29 (m, 4H), 1.02 (d, 3H), 0.98 (d, 6H).

[0055] S3. Add 0.1 mol of the intermediate and 0.4 mol of potassium carbonate to 250 mL of dimethyl sulfoxide, add 0.115 mol of caprolactam, heat to 80°C, stir to react for 1.5 hours, cool to room temperature, filter, and recrystallize from toluene to obtain the product. ESI-MS calculated value: C 29 H 46 NO 4 (M+H) + 472.33, found: 472.3, yield: 79%.

[0056] NMR results: 1 H NMR (300 MHz, CDCl 3)δ7.90(d, J=6.7Hz, 1H), 7.40(m, 1H), 6.87-6.90(m, 2H), 3.93(m, 3H), 3.35(t, 2H), 3.21(t, 2H), 2.18(t, 2H), 2.04( m, 1H), 1.80 (m, 3H), 1.74 (m, 2H), 1.55-1.60 (m, 7H), 1.41-1.44 (m, 4H), 1.28-1.31 (m, 6H), 1.02 (d, 3H), 0.98 (d, 6H).

[0057] Preparation Example 2 Preparation method of algae protein peptide

[0058] The details are as follows:

[0059] T1 5 parts by weight of Spirulina, 2 parts by weight of Chlorella pyrenoidosa were dried, crushed, and mixed to obtain algae powder;

[0060] T2. The algae powder prepared in step T1 is added to water, wherein the solid-liquid ratio of the algae powder to water is 1:5 g / mL, and ultrasonically heated to 40°C with a power of 1200 W, extracted for 2 hours, filtered, the solid is retained, and the filtrate is freeze-dried to obtain algae pigment protein;

[0061] T3. Add 100 parts by weight of the solid in step T2 to water, add 1 part by weight of the complex enzyme, inoculate Lactobacillus reuteri seed solution, the inoculation amount is 2v / v%, under anoxic conditions, 35°C, 100r / min, enzymatic fermentation culture for 24h, filter, dialyze the filtrate with a dialysis bag with a pore size of 5kDa for 2h, and freeze-dry the permeate to obtain a small molecule algae protein peptide;

[0062] The complex enzyme includes cellulase and papain in a mass ratio of 7:2;

[0063] T4. 10 parts by weight of the phycocyanin protein prepared in step T2 and 7 parts by weight of the small molecule phycocyanin peptide prepared in step T3 are mixed evenly to prepare phycocyanin peptide.

[0064] Preparation Example 3 Preparation method of algae protein peptide

[0065] The details are as follows:

[0066] T1 7 parts by weight of Spirulina, 4 parts by weight of Chlorella pyrenoidosa were dried, crushed, and mixed to obtain algae powder;

[0067] T2. The algae powder prepared in step T1 is added to water, wherein the solid-liquid ratio of the algae powder to water is 1:7 g / mL, and ultrasonically heated to 50°C with a power of 1500 W, extracted for 4 hours, filtered, the solid is retained, and the filtrate is freeze-dried to obtain algae pigment protein;

[0068] T3. Add 100 parts by weight of the solid in step T2 to water, add 2 parts by weight of complex enzyme, inoculate Lactobacillus reuteri seed solution, inoculation amount is 4v / v%, under anoxic conditions, 40°C, 120r / min, enzymatic fermentation culture for 36h, filter, dialyze the filtrate with a dialysis bag with a pore size of 7kDa for 4h, freeze-dry the permeate to obtain a small molecule algae protein peptide;

[0069] The complex enzyme includes cellulase and papain in a mass ratio of 10:4;

[0070] T4. 12 parts by weight of the phycocyanin protein prepared in step T2 and 10 parts by weight of the small molecule phycocyanin peptide prepared in step T3 are mixed evenly to prepare phycocyanin peptide.

[0071] Preparation Example 4 Preparation method of algae protein peptide

[0072] The details are as follows:

[0073] T1 6 parts by weight of Spirulina, 3 parts by weight of Chlorella pyrenoidosa dried, crushed, mixed, to obtain algae powder;

[0074] T2. The algae powder prepared in step T1 is added to water, wherein the solid-liquid ratio of the algae powder to water is 1:6 g / mL, and ultrasonically heated to 45°C with a power of 1350 W, extracted for 3 hours, filtered, the solid is retained, and the filtrate is freeze-dried to obtain algae pigment protein;

[0075] T3. Add 100 parts by weight of the solid in step T2 to water, add 1.5 parts by weight of the complex enzyme, inoculate with Lactobacillus reuteri seed solution, inoculation amount of 3v / v%, under anoxic conditions, 37°C, 110r / min, enzymatic fermentation culture for 30h, filter, dialyze the filtrate with a dialysis bag with a pore size of 6kDa for 3h, and freeze-dry the permeate to obtain a small molecule algae protein peptide;

[0076] The complex enzyme includes cellulase and papain in a mass ratio of 8:3;

[0077] T4. 11 parts by weight of the phycocyanin protein prepared in step T2 and 8.5 parts by weight of the small molecule phycocyanin peptide prepared in step T3 were mixed evenly to prepare phycocyanin peptide.

[0078] Preparation Example 5

[0079] Compared with Preparation Example 4, the difference is that the composite enzyme is a single cellulase.

[0080] Preparation Example 6

[0081] Compared with Preparation Example 4, the difference is that the composite enzyme is a single papain.

[0082] Comparative Preparation Example 1

[0083] Compared with Preparation Example 4, the difference is that Spirulina is not added in step T1.

[0084] Comparative Preparation Example 2

[0085] Compared with Preparation Example 4, the difference is that no Chlorella pyrenoidosa is added in step T1.

[0086] Comparative Preparation Example 3

[0087] Compared with Preparation Example 4, the difference is that no complex enzyme is added in step T3.

[0088] Comparative Preparation Example 4

[0089] Compared with Preparation Example 4, the difference is that no phycocyanin is added in step T4.

[0090] Comparative Preparation Example 5

[0091] Compared with Preparation Example 4, the difference is that no small molecule algae protein peptide is added in step T4.

[0092] Example 1

[0093] This embodiment provides a method for preparing an anti-aging cosmetic, comprising the following steps:

[0094] (1) The novel permeation enhancer prepared in Preparation Example 1 and glycerol were mixed in a mass ratio of 5:1 to prepare a permeation enhancer composition;

[0095] (2) The algae protein peptide, blue copper peptide and acetyl tetrapeptide prepared in Preparation Example 2 were mixed in a mass ratio of 15:3:1 to prepare a composite peptide composition;

[0096] (3) dissolving 3 parts by weight of β-nicotinamide mononucleotide, 1 part by weight of ergothioneine, and 1 part by weight of the composite peptide composition in purified water, stirring and mixing for 15 minutes to obtain an aqueous phase;

[0097] (4) adding 0.1 parts by weight of the penetration enhancer composition to 3 parts by weight of grape seed oil, stirring and mixing for 15 minutes to obtain an oil phase;

[0098] (5) The aqueous phase and the oil phase were mixed, 0.3 parts by weight of carbomer was added, emulsified at 6000 r / min for 15 min, and filtered to prepare an anti-aging cosmetic.

[0099] Example 2

[0100] This embodiment provides a method for preparing an anti-aging cosmetic, comprising the following steps:

[0101] (1) The novel permeation enhancer prepared in Preparation Example 1 and propylene glycol were mixed in a mass ratio of 7:2 to prepare a permeation enhancer composition;

[0102] (2) The algae protein peptide, blue copper peptide and acetyl tetrapeptide prepared in Preparation Example 3 were mixed in a mass ratio of 20:5:2 to prepare a composite peptide composition;

[0103] (3) dissolving 5 parts by weight of β-nicotinamide mononucleotide, 2 parts by weight of ergothioneine, and 2 parts by weight of the composite peptide composition in purified water, stirring and mixing for 15 minutes to obtain an aqueous phase;

[0104] (4) adding 0.2 parts by weight of the penetration enhancer composition to 5 parts by weight of grape seed oil, stirring and mixing for 15 minutes to obtain an oil phase;

[0105] (5) The aqueous phase and the oil phase were mixed, 0.5 parts by weight of carbomer was added, emulsified at 6000 r / min for 15 min, and filtered to prepare an anti-aging cosmetic.

[0106] Example 3

[0107] This embodiment provides a method for preparing an anti-aging cosmetic, comprising the following steps:

[0108] (1) The novel permeation enhancer prepared in Preparation Example 1 and glycerol were mixed in a mass ratio of 6:1.5 to prepare a permeation enhancer composition;

[0109] (2) The algae protein peptide, blue copper peptide and acetyl tetrapeptide prepared in Preparation Example 4 were mixed in a mass ratio of 17:4:1.5 to prepare a composite peptide composition;

[0110] (3) dissolving 4 parts by weight of β-nicotinamide mononucleotide, 1.5 parts by weight of ergothioneine, and 1.5 parts by weight of the composite peptide composition in purified water, stirring and mixing for 15 minutes to obtain an aqueous phase;

[0111] (4) adding 0.15 parts by weight of the penetration enhancer composition to 4 parts by weight of grape seed oil, stirring and mixing for 15 minutes to obtain an oil phase;

[0112] (5) The aqueous phase and the oil phase were mixed, 0.4 parts by weight of carbomer was added, emulsified at 6000 r / min for 15 min, and filtered to prepare an anti-aging cosmetic.

[0113] Embodiment 4-5

[0114] Compared with Example 3, the difference is that the algae protein peptides are prepared by Preparation Examples 5 and 6 respectively.

[0115] Comparative Examples 1-5

[0116] Compared with Example 3, the difference is that the algae protein peptides are prepared by comparative preparation examples 1-5 respectively.

[0117] Comparative Example 6

[0118] Compared with Example 3, the difference is that the permeation enhancer composition includes a single novel permeation enhancer.

[0119] Comparative Example 7

[0120] Compared with Example 3, the difference lies in that the penetration enhancer composition includes only glycerol.

[0121] Comparative Example 8

[0122] Compared with Example 3, the difference is that no penetration enhancer composition is added.

[0123] Comparative Example 9

[0124] Compared with Example 3, the difference is that no algae protein peptide is added.

[0125] Comparative Example 10

[0126] Compared with Example 3, the difference is that β-nicotinamide mononucleotide is not added.

[0127] Comparative Example 11

[0128] Compared with Example 3, the difference is that thioneine is not added.

[0129] Comparative Example 12

[0130] Compared with Example 3, the difference is that β-nicotinamide mononucleotide and ergothioneine are not added.

[0131] Test Example 1 Human skin patch test and allergy test

[0132] Test samples: anti-aging cosmetics prepared in Examples 1-5 and Comparative Examples 1-12 of the present invention.

[0133] Experimental method: Subjects aged 20-59 were selected and randomly divided into 17 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 1-17 spot tester holes, respectively, with a dosage of 10-20μL. Bathing was prohibited during the test, and the normal reaction was negative. The test samples were distributed to the subjects and acted on the face, neck and back of the ears of the subjects. The skin condition of the subjects was observed after 10 minutes. The experimental results are shown in Table 1.

[0134] Table 1

[0135] 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

[0136] As can be seen from the above table, the patch reactions of the anti-aging cosmetics prepared in Examples 1-5 of the present invention and Comparative Examples 1-12 are negative reactions, and they are safe to use without any allergic reactions.

[0137] Test Example 2

[0138] The anti-aging cosmetics prepared in Examples 1-5 and Comparative Examples 1-12 were diluted 1000 times with purified water to prepare sample solutions.

[0139] 1. DPPH free radical scavenging rate test method:

[0140] Take 1mL of 2mmol / L DPPH (1,1-diphenyl-2-trinitrophenylhydrazine) working solution and place it in a test tube. 1 1 mL of sample solution was added to the blank group (the result was expressed as A 2 Purified water was used to replace the DPPH working solution; negative control group (results were expressed as A 3 (denoted by) using purified water instead of working solution. Mix all reagents evenly, keep away from light for 30 minutes, repeat the test 3 times, use ultraviolet spectrophotometer to measure absorbance at 517nm, and take the average value to calculate the scavenging rate. The calculation formula of DPPH free radical scavenging rate is:

[0141] DPPH free radical scavenging rate (%) = [1-(A 2 -A 1 ) / A 3 ]×100%

[0142] 2. ABTS + Free radical scavenging rate determination method

[0143] 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 test well (results were expressed as A 0 The sample solution was replaced with purified water; the control test well (the result was expressed as A j Phosphate buffer solution (pH 6.7) (used to prepare ABTS + Working fluid) instead of ABTS + Working solution. After mixing, place the kit at room temperature and away from light for 8 minutes, and use a UV 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:

[0144] ABTS + Base clearance rate (%) = [1-(A i -A j ) / A 0 ]×100%

[0145] The results are shown in Table 2.

[0146] Table 2

[0147]

[0148]

[0149] It can be seen from the above table that the anti-aging cosmetics prepared in Examples 1-3 of the present invention have good antioxidant effects.

[0150] Test Example 3

[0151] Female subjects aged 19-53 were selected on a voluntary basis and randomly divided into 17 groups, each with 6 people, namely, Example 1-5 and Comparative Example 1-12. During the test, no drugs or cosmetics irrelevant to the test were applied, and the samples were applied on both sides of the face of the subjects. The sample group used the anti-aging cosmetics prepared in Example 1-5 and Comparative Example 1-12. Once a day for 2 weeks, before the test, the subjects washed the test area with clean water, wiped it dry, and sat quietly for 20 minutes in a constant environment of 25±1°C and relative humidity of 45±5%.

[0152] 1. Skin moisturizing test

[0153] The stratum corneum moisture content was measured before the test, and the stratum corneum moisture content of the subjects was tested 1 hour after using the sample on the 14th day, and the skin moisture content change rate (%) was calculated. The stratum corneum moisture content of the test site was tested using a skin moisture tester, and the average value was taken for 5 times.

[0154] Skin moisture content change rate (%) = (moisture content after use - moisture content before use) / moisture content before use × 100%

[0155] 2. Skin elasticity test

[0156] The skin elasticity and roughness parameters were tested before the start of the test. On the 14th day, 1 hour after using the sample, the stratum corneum water content of the subjects was tested and the skin water content change rate (%) was calculated. The skin elasticity and roughness parameters of the test site were tested using a skin elasticity tester and the average value was taken for 5 times.

[0157] Skin elasticity change rate (%) = (skin elasticity after use - skin elasticity before use) / skin elasticity before use × 100%

[0158] Roughness change rate (%) = (roughness after use - roughness before use) / roughness before use × 100%

[0159] The results are shown in Table 3.

[0160] Table 3

[0161] Group Skin moisture content change rate (%) Skin elasticity change rate (%) Roughness change rate (%) Example 1 27.24 18.25 -20.11 Example 2 27.04 18.45 -19.58 Example 3 28.57 19.05 -21.44 Example 4 24.56 15.66 -16.02 Example 5 24.98 15.19 -15.86 Comparative Example 1 22.58 14.02 -13.89 Comparative Example 2 23.09 14.17 -14.08 Comparative Example 3 23.25 14.58 -14.55 Comparative Example 4 22.10 13.11 -13.58 Comparative Example 5 20.59 11.58 -11.29 Comparative Example 6 21.52 13.25 -14.56 Comparative Example 7 23.59 15.62 -16.09 Comparative Example 8 19.25 10.88 -12.28 Comparative Example 9 18.52 10.25 -10.25 Comparative Example 10 16.26 11.57 -12.56 Comparative Example 11 18.24 12.93 -11.37 Comparative Example 12 14.52 9.28 -10.07

[0162] It can be seen from the above table that the anti-aging cosmetics prepared in Examples 1-3 of the present invention have good moisturizing effect and the effects of increasing skin elasticity and reducing skin roughness.

[0163] 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. An anti-aging cosmetic, characterized in that: The method is prepared from the following raw materials in parts by weight: 3-5 parts of β-nicotinamide mononucleotide, 1-2 parts of ergothioneine, 0.1-0.2 parts of a penetration enhancer composition, 0.3-0.5 parts of carbomer, 1-2 parts of a composite peptide composition, 3-5 parts of grape seed oil and 15-20 parts of purified water; The penetration enhancer composition is composed of a novel penetration enhancer and a small molecule alcohol in a mass ratio of 5-7:1-2. The structural formula of the novel penetration enhancer is shown in Formula I: Wherein, R = C6-C12 alkyl chain; The composite peptide composition is composed of algae protein peptide, blue copper peptide and acetyl tetrapeptide, and the mass ratio is 15-20:3-5:1-2; The preparation method of the novel penetration enhancer is as follows: S1. reacting menthol and salicylic acid to obtain menthol salicylate; S2. Menthol salicylate and dihaloalkane are reacted to obtain an intermediate having the following structure: S3. reacting the intermediate with caprolactam to obtain a product; The preparation method of the algae protein peptide is as follows: T1. The Spirulina and Chlorella pyrenoidosa were dried, crushed, and mixed to obtain algae powder; T2. Add the algae powder obtained in step T1 to water, extract by ultrasonic heating, filter, retain the solid, and freeze-dry the filtrate to obtain algae pigment protein; T3. The solid in step T2 is added to water, a composite enzyme is added, the seed solution of Lactobacillus reuteri is inoculated, enzymatic fermentation is performed, filtration is performed, the filtrate is dialyzed, and the permeate is freeze-dried to obtain a small molecule algae protein peptide; T4. Evenly mix the phycocyanin protein obtained in step T2 and the small molecule phycocyanin peptide obtained in step T3 to obtain phycocyanin peptide.

2. The anti-aging cosmetic according to claim 1, characterized in that: The small molecule alcohol is selected from at least one of glycerol, propylene glycol, butylene glycol and ethanol.

3. The anti-aging cosmetic according to claim 1, characterized in that: The molar ratio of menthol to salicylic acid in step S1 is 1:1-1.15; the molar ratio of menthol salicylate to dihaloalkane in step S2 is 1.1-1.2:1, the reaction temperature is 50-60°C, the reaction time is 2-4h, and the dihaloalkane is selected from 1,6-dichlorohexane, 1,6-dibromohexane, 1,7-dichloroheptane, 1,7-dibromoheptane, 1,8-dichlorooctane, 1,8-dibromo At least one of octane, 1,9-dichlorononane, 1,9-dibromononane, 1,10-dichlorodecane, 1,10-dibromodecane, 1,11-dichloroundecane, 1,11-dibromodecane, 1,12-dichlorododecane and 1,12-dibromodecane; the molar ratio of the intermediate to caprolactam in step S3 is 1:1.1-1.2, the reaction temperature is 75-85°C, and the reaction time is 1-2h.

4. The anti-aging cosmetic according to claim 1, characterized in that: The preparation method of the novel penetration enhancer is specifically as follows: S1. Add 1 molar equivalent of menthol and 1-1.15 molar equivalent of salicylic acid to toluene, add 2-4wt% concentrated sulfuric acid based on the total mass of the system, heat to reflux, stir to react for 5-7h, cool to room temperature, filter, wash, and dry to obtain menthol salicylate; S2. 1.1-1.2 molar equivalents of menthol salicylate and 3-5 molar equivalents of triethylamine are added to acetonitrile, 1 molar equivalent of dihaloalkane is added, heated to 50-60°C, stirred for 2-4h, cooled to room temperature, filtered, washed, and recrystallized from ethyl acetate to obtain an intermediate; S3. Add 1 molar equivalent of the intermediate and 3-5 molar equivalents of potassium carbonate to dimethyl sulfoxide, add 1.1-1.2 molar equivalents of caprolactam, heat to 75-85°C, stir to react for 1-2h, cool to room temperature, filter, and recrystallize from toluene to obtain the product.

5. The anti-aging cosmetic according to claim 1, characterized in that: The mass ratio of Spirulina to Chlorella pyrenoidosa in step T1 is 5-7:2-4; the ultrasonic power in the ultrasonic heating extraction in step T2 is 1200-1500W, the heating temperature is 40-50°C, the time is 2-4h, and the solid-liquid ratio of the algae powder and water is 1:5-7g / mL; the mass ratio of the solid, water, and complex enzyme in step T3 is 10-12:100:1-2, the complex enzyme includes cellulase and papain, the mass ratio is 7-10:2-4, the inoculation amount of the Lactobacillus reuteri seed liquid is 2-4v / v%, and the bacterial content of the Lactobacillus reuteri seed liquid is 10 7 -10 8 cfu / mL, the conditions of the enzymatic fermentation are under anoxic conditions, 35-40°C, 100-120r / min, the enzymatic fermentation culture is 24-36h, the dialysis bag pore size used in the dialysis is 5k-7kDa, and the dialysis time is 2-4h; the mass ratio of the algae pigment protein and the small molecule algae protein peptide in step T4 is 10-12:7-10.

6. The anti-aging cosmetic according to claim 1, characterized in that: The preparation method of the algae protein peptide is specifically as follows: T1 5-7 parts by weight of Spirulina, 2-4 parts by weight of Chlorella pyrenoidosa dried, crushed, mixed, to obtain algae powder; T2. The algae powder prepared in step T1 is added to water, wherein the solid-liquid ratio of the algae powder to water is 1:5-7 g / mL, and ultrasonically heated to 40-50°C with a power of 1200-1500 W, extracted for 2-4 hours, filtered, the solid is retained, and the filtrate is freeze-dried to obtain algae pigment protein; T3. Add 100 parts by weight of the solid in step T2 into water, add 1-2 parts by weight of the complex enzyme, and inoculate the bacterial content to 10 7 -10 8 cfu / mL of Lactobacillus reuteri seed solution, inoculation amount of 2-4v / v%, under anoxic conditions, 35-40°C, 100-120r / min, enzymatic fermentation culture for 24-36h, filtration, filtration of the filtrate with a dialysis bag with a pore size of 5k-7kDa for 2-4h, freeze-drying the permeate to obtain small molecule algae protein peptides; The complex enzyme comprises cellulase and papain in a mass ratio of 7-10:2-4; T4. 10-12 parts by weight of the phycocyanin protein prepared in step T2 and 7-10 parts by weight of the small molecule phycocyanin peptide prepared in step T3 are mixed evenly to prepare phycocyanin peptide.

7. A method for preparing the anti-aging cosmetic according to any one of claims 1 to 6, characterized in that: The following steps are involved: (1) dissolving β-nicotinamide mononucleotide, ergothioneine, and the composite peptide composition in purified water, stirring and mixing to obtain an aqueous phase; (2) adding the penetration enhancer composition to the grape seed oil, stirring and mixing uniformly to obtain an oil phase; (3) The water phase and the oil phase are mixed, carbomer is added, emulsified, filtered, and the anti-aging cosmetic is prepared.

8. Use of the anti-aging cosmetic according to any one of claims 1 to 6 in the preparation of products that promote skin repair, anti-aging, anti-allergy, and improve skin elasticity.

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