WO2023024289A1 - 一种具有美白功效的组合物及其制备方法和应用 - Google Patents

一种具有美白功效的组合物及其制备方法和应用 Download PDF

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WO2023024289A1
WO2023024289A1 PCT/CN2021/132449 CN2021132449W WO2023024289A1 WO 2023024289 A1 WO2023024289 A1 WO 2023024289A1 CN 2021132449 W CN2021132449 W CN 2021132449W WO 2023024289 A1 WO2023024289 A1 WO 2023024289A1
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acid
composition
parts
derivatives
comparative
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PCT/CN2021/132449
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English (en)
French (fr)
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孔秋婵
陈庆生
夏高辉
毛善巧
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广州环亚化妆品科技股份有限公司
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Publication of WO2023024289A1 publication Critical patent/WO2023024289A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34—Alcohols
    • A61K8/347—Phenols
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/368—Carboxylic acids; Salts or anhydrides thereof with carboxyl groups directly bound to carbon atoms of aromatic rings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67—Vitamins
    • A61K8/676—Ascorbic acid, i.e. vitamin C
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions
    • A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/74—Biological properties of particular ingredients
    • A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782—Enzyme inhibitors; Enzyme antagonists

Definitions

  • the invention belongs to the technical field of cosmetics, and in particular relates to a composition with whitening effect and its preparation method and application.
  • the whitening products on the market have a single whitening effect, only targeting part of the process of melanin production, and the whitening effect is weak.
  • more cosmetic companies are considering using plant-based ingredients instead of synthetic whitening agents.
  • this method not only cannot ensure the safety of the product but also reduces the effectiveness of the product.
  • the existing related art discloses a whitening and blemish-relieving composition and its application.
  • the whitening and blemish-relieving composition includes the following raw materials: egg yolk, shea butter, pterostilbene, vitamin E, hydrolyzed ceramide III, orange peel extract extract, yeast extract, thyme extract, white willow bark extract, mullein extract, crinoid neuroactive whitening factor, baicalin extract, oxidized resveratrol, lactobacillus fermentation lysate, tranexamic acid, VC B base ether, water-soluble fullerene, 4-butylresorcinol and ectoine.
  • This invention inhibits the production of melanin to a certain extent, but the whitening effect is not obvious.
  • the related art discloses a skin brightening and whitening traditional Chinese medicine composition, a skin brightening and whitening traditional Chinese medicine preparation, a skin brightening and whitening facial mask, and a preparation method.
  • the traditional Chinese medicine composition is composed of the following raw materials in parts by weight: 2-4 parts of Forsythia fruit extract, 3-5 parts of Fangfeng extract, 2-4 parts of safflower extract, 3-5 parts of licorice root extract, angelica Extract 2-4 parts, Salvia miltiorrhiza extract 2-4 parts, Comfrey root extract 2-4 parts, Bletilla striata extract 2-4 parts, peach kernel extract 3-5 parts, Ginkgo biloba extract 3-5 parts, water soluble 1-3 parts of pearl powder.
  • the traditional Chinese medicine prescription has the effects of promoting blood circulation and removing blood stasis, filling qi and blood, making people's complexion ruddy, diluting dullness, and enhancing luster, but the effects of whitening and diluting stains are relatively weak.
  • the present invention aims to solve at least one of the technical problems in the above-mentioned prior art. Therefore, the present invention proposes a composition with whitening effect and its preparation method and application.
  • the composition with whitening effect is mild and safe, and can achieve rapid whitening effect.
  • the first aspect of the present invention provides a composition with whitening effect
  • the composition includes the following components: ⁇ -hydroxy acid, resorcinol derivatives, ascorbic acid and its derivatives, tranexamic acid and gallic acid and its derivatives things.
  • ⁇ -hydroxy acid refers to a series of carboxylic acids with a hydroxyl group in the ⁇ position, commonly known as fruit acid, ⁇ -hydroxy acid can peel off the aging cuticle, promote the metabolism and degradation of epidermal melanin, improve skin dullness, hyperpigmentation, and make the skin whitening.
  • Gallic acid is a powerful tyrosinase inhibitor and an excellent antioxidant, which can effectively inhibit the transfer of melanin and achieve whitening effect. At the same time, gallic acid can also prevent DNA damage and inhibit skin inflammation.
  • Resorcinol derivatives have super strong inhibitory tyrosinase activity, thereby inhibiting the synthesis of melanin. They are very effective skin whitening agents, which can also work at very low concentrations. Among them, phenylethyl isophthalic acid Phenol is one of the most active tyrosinase inhibitors reported among resorcinol derivatives.
  • Ascorbic acid and its derivatives are safe and effective skin whitening agents. Ascorbic acid and its derivatives participate in the metabolism of tyrosinase in the body, promote the oxidation and decomposition of tyrosinase in the body, and reduce the conversion of tyrosine into melanin. Ascorbic acid and its derivatives also have potential anti-inflammatory activity, which can promote wound healing and prevent post-inflammatory hyperpigmentation. Among them, ascorbic acid ethyl ether is the best derivative of ascorbic acid so far. It not only has a stable structure but also can be absorbed through the skin with high bioavailability.
  • Tranexamic acid prevents pigmentation caused by ultraviolet rays by interfering with the structure of plasminogen and preventing the combination of plasminogen and keratinocyte lysine sites, so as to achieve the effect of lightening spots. Tranexamic acid has high safety, few adverse reactions, good curative effect, and has good therapeutic effect on chloasma.
  • Enhance metabolism ⁇ -hydroxy acid enhances skin metabolism, promotes the metabolism and degradation of epidermal melanin, immediately improves skin gloss and softness, and promotes the absorption of other ingredients;
  • gallic acid and its derivatives can effectively inhibit the transfer of melanin (galactose receptor ligand in keratinocytes, involved in the process of transferring melanin from melanocytes to keratinocytes), to achieve whitening effect;
  • Inhibition of production Inhibition of tyrosinase activity by resorcinol derivatives, ascorbic acid and its derivatives to promote tyrosinase oxidation decomposition and tranexamic acid interference with plasmin activity and other three ways to inhibit the synthesis of melanin, to achieve Whitening effect.
  • composition prepared by the invention has fast, effective and long-lasting whitening effect.
  • the composition also includes an antisensitizer, a polyol and deionized water, and the parts by weight of each component are as follows: 0.1-10 parts of ⁇ -hydroxy acid, 0.01-1 part of resorcinol derivatives, ascorbic acid and 0.1-10 parts of its derivatives, 0.1-10 parts of tranexamic acid, 0.01-1 parts of gallic acid and its derivatives, 0.01-0.1 parts of antisensitivity agent, 5-10 parts of polyols, and 60-90 parts of deionized water.
  • an antisensitizer a polyol and deionized water
  • the parts by weight of each component are as follows: 0.1-10 parts of ⁇ -hydroxy acid, 0.01-1 part of resorcinol derivatives, ascorbic acid and 0.1-10 parts of its derivatives, 0.1-10 parts of tranexamic acid, 0.01-1 parts of gallic acid and its derivatives, 0.01-0.1 parts of antisensitivity agent, 5-10 parts of polyols, and 60-90 parts
  • the parts by weight of each component are as follows: 1-10 parts of ⁇ -hydroxy acid, 0.01-0.5 parts of resorcinol derivatives, 0.1-10 parts of vitamin C and its derivatives, 0.1-10 parts of tranexamic acid, gall 0.05-1 part of acid and its derivative, 0.01-0.1 part of antisensitizer, 5-10 part of polyol, 60-90 part of deionized water.
  • the parts by weight of each component are as follows: 1-10 parts of ⁇ -hydroxy acid, 0.01-0.5 parts of resorcinol derivatives, 5-10 parts of vitamin C and its derivatives, 0.1-10 parts of tranexamic acid, gall 0.05-1 part of acid and its derivatives, 0.01-0.1 part of antisensitizer, 0.01-0.1 part of antisensitizer, 5-10 parts of polyol, 60-90 parts of deionized water.
  • the parts by weight of each component are as follows: 1-10 parts of ⁇ -hydroxy acid, 0.01-0.5 parts of resorcinol derivatives, 5-10 parts of vitamin C and its derivatives, 0.1-5 parts of tranexamic acid, gall 0.1-0.5 parts of acid and its derivatives, 0.01-0.1 part of antisensitizer, 0.01-0.1 part of antisensitizer, 5-10 parts of polyol, 60-90 parts of deionized water.
  • the ⁇ -hydroxy acid includes at least one of lactic acid, glycolic acid, citric acid, malic acid, tartaric acid and mandelic acid. More preferably, the alpha-hydroxy acid is a mixture of lactic acid, glycolic acid, citric acid, malic acid, tartaric acid and mandelic acid. Most preferably, the ⁇ -hydroxy acid is lactic acid, glycolic acid, citric acid, malic acid, tartaric acid and mandelic acid in a mass ratio of 1: (0.5-1.5): (0.1-0.5): (0.01-0.1): (0.01-0.1): (0.01-0.1) mixed mixture.
  • the resorcinol derivatives include 4-butylresorcinol, hexylresorcinol, phenethylresorcinol, dimethoxycresyl-4-propylresorcinol at least one of the
  • the ascorbic acid and its derivatives include at least one of ascorbic acid, sodium ascorbyl phosphate, magnesium ascorbyl phosphate, ascorbyl glucoside, and ascorbyl ethyl ether.
  • the gallic acid and its derivatives include at least one of diglucosyl gallic acid, gallic acid, propyl gallate, ethylhexyl gallate, and ellagic acid.
  • the antisensitizing agent includes at least one of hydroxyphenylpropanamide benzoic acid, madecassoside, paeonol, and ⁇ -glucan.
  • Hydroxyphenylpropanamide benzoic acid is an effective anti-itch and anti-sensitivity agent in cosmetics. It can exert multiple functions such as anti-histamine, anti-oxidation, anti-irritation, anti-inflammation, and improvement of erythema. Good effect on red.
  • the addition of hydroxyphenylpropanamide benzoic acid to the composition of the present invention makes the composition safer and milder and avoids irritation.
  • Madecassoside is a triterpenoid saponin component contained in Centella asiatica. It has anti-oxidation, antibacterial, and immune-regulating functions. It can increase the resistance of the skin and epidermis. Improves skin elasticity, enhances skin softness, and delays aging.
  • Paeonol has anti-inflammatory effect and has preventive effect on various skin diseases.
  • ⁇ -glucan has significant anti-inflammatory and anti-allergic activities, which can reduce skin allergies and inflammation.
  • the present invention can effectively suppress the stress response that may be caused by the composition by additionally adding anti-allergic ingredients, making the product safer and milder.
  • the polyhydric alcohol is at least one of 1,3-propanediol, glycerin, 1,2-pentanediol, and 1,2-hexanediol.
  • the second aspect of the present invention provides the preparation method of the composition with whitening effect, comprising the following steps:
  • the components are mixed to obtain the composition with whitening effect.
  • the preparation method of the composition with whitening effect comprises the following steps:
  • the addition of the antisensitizer needs to be based on the solubility of the actually selected substance, and which step is specifically selected for addition.
  • Phenylpropanamide benzoic acid is dissolved in polyols in step (1); madecassoside is selected as the antisensitizer, and madecassoside is dissolved in deionized water in step (2).
  • the third aspect of the present invention provides the application of the composition with whitening effect in cosmetics.
  • a cosmetic comprising the composition with whitening effect and auxiliary materials described in the present invention.
  • a facial mask includes the composition with whitening effect and auxiliary materials described in the present invention.
  • the auxiliary materials include at least one of preservatives, moisturizing agents and thickeners.
  • composition with whitening effect of the present invention ⁇ -hydroxy acid, resorcinol derivatives, ascorbic acid and its derivatives, tranexamic acid, gallic acid and their derivatives are used in combination, and each component complements and synergizes , acts on the skin from three dimensions to achieve fast, effective and long-lasting whitening.
  • the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial channels, or can be obtained by existing known methods.
  • a composition with whitening effect comprising the following components in parts by weight: 5 parts of ⁇ -hydroxy acid, 0.2 part of phenylethyl resorcinol, 5 parts of ethyl ascorbic acid, 5 parts of tranexamic acid, diglucose 0.3 parts of gallic acid, 0.03 parts of hydroxyphenylpropionamide benzoic acid, 5 parts of 1,2-pentanediol, and 79.47 parts of deionized water.
  • the ⁇ -hydroxy acid is a mixture of lactic acid, glycolic acid, citric acid, malic acid, tartaric acid and mandelic acid in a mass ratio of 1:1:0.3:0.05:0.05:0.05.
  • a composition with whitening effect comprising the following components in parts by weight: 2 parts of ⁇ -hydroxy acid, 0.5 part of hexylresorcinol, 1 part of sodium ascorbyl phosphate, 3 parts of tranexamic acid, and 0.3 part of ellagic acid , 0.05 parts of madecassoside, 10 parts of glycerin, and 83.15 parts of deionized water.
  • the alpha-hydroxy acid is a mixture of citric acid, malic acid, tartaric acid and mandelic acid in a mass ratio of 0.3:0.05:0.05:0.05.
  • a composition with whitening effect comprising the following components in parts by weight: 10 parts of ⁇ -hydroxy acid, 0.1 part of 4-butyl resorcinol, 1 part of ascorbic acid glucoside, 1 part of tranexamic acid, and propyl gallate 0.5 parts of esters, 0.02 parts of paeonol, 5 parts of 1,3-propanediol, and 82.38 parts of deionized water.
  • the ⁇ -hydroxy acid is a mixture of lactic acid, glycolic acid, citric acid, malic acid and mandelic acid in a mass ratio of 1:1:0.3:0.05:0.05.
  • a composition with whitening effect comprising the following components in parts by weight: 5 parts of ⁇ -hydroxy acid, 0.2 part of phenylethyl resorcinol, 5 parts of ethyl ascorbic acid, 5 parts of tranexamic acid, diglucose 0.3 parts of gallic acid, 5 parts of 1,2-pentanediol, and 79.5 parts of deionized water.
  • the ⁇ -hydroxy acid is a mixture of lactic acid and glycolic acid in a mass ratio of 1:1.
  • Example 1 Compared with Example 1, in Comparative Example 1, phenylethyl resorcinol, ascorbic acid ethyl ether, tranexamic acid and diglucosyl gallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 2 Compared with Example 1, in Comparative Example 2, the ⁇ -hydroxy acid was replaced by deionized water, and other conditions were the same as in Example 1.
  • Example 3 Compared with Example 1, in Comparative Example 3, ⁇ -hydroxy acid, ascorbic acid ethyl ether, tranexamic acid and diglucosylgallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 4 Compared with Example 1, in Comparative Example 4, phenylethylresorcinol was replaced by deionized water, and other conditions were the same as in Example 1.
  • Example 1 Compared with Example 1, in Comparative Example 5, ⁇ -hydroxy acid, phenylethylresorcinol, tranexamic acid and diglucosylgallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 6 Compared with Example 1, ascorbic acid ethyl ether was replaced by deionized water in Comparative Example 6, and other conditions were the same as in Example 1.
  • Example 7 Compared with Example 1, in Comparative Example 7, ⁇ -hydroxy acid, phenylethylresorcinol, ascorbic acid ethyl ether and diglucosyl gallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 8 Compared with Example 1, in Comparative Example 8, tranexamic acid was replaced by deionized water, and other conditions were the same as in Example 1.
  • Example 9 Compared with Example 1, in Comparative Example 9, ⁇ -hydroxy acid, phenylethyl resorcinol, ascorbic acid ethyl ether and tranexamic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 10 Compared with Example 1, diglucosylgallic acid was replaced with deionized water in Comparative Example 10, and other conditions were the same as in Example 1.
  • Example 11 Compared with Example 1, in Comparative Example 11, ⁇ -hydroxy acid and phenylethylresorcinol were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 12 Compared with Example 1, in Comparative Example 12, ⁇ -hydroxy acid and ascorbic acid ethyl ether were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 13 Compared with Example 1, in Comparative Example 13, ⁇ -hydroxy acid and tranexamic acid were replaced by deionized water, and other conditions were the same as Example 1.
  • Example 14 Compared with Example 1, in Comparative Example 14, ⁇ -hydroxy acid and diglucosylgallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 15 Compared with Example 1, in Comparative Example 15, ⁇ -hydroxy acid and hydroxyphenylpropionamide benzoic acid were replaced by deionized water, and other conditions were the same as in Example 1.
  • Example 16 Compared with Example 1, in Comparative Example 16, phenylethyl resorcinol and ascorbic acid ethyl ether were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 17 Compared with Example 1, in Comparative Example 17, phenylethylresorcinol and tranexamic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 18 Compared with Example 1, in Comparative Example 18, phenylethyl resorcinol and diglucosyl gallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 19 Compared with Example 1, in Comparative Example 19, phenylethylresorcinol and hydroxyphenylpropionamide benzoic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 20 Compared with Example 1, in Comparative Example 20, ascorbic acid ethyl ether and tranexamic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 21 Compared with Example 1, in Comparative Example 21, ascorbic acid ethyl ether and diglucosyl gallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 22 Compared with Example 1, in Comparative Example 22, ascorbic acid ethyl ether and hydroxyphenylpropionamide benzoic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 23 Compared with Example 1, in Comparative Example 23, tranexamic acid and diglucosylgallic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 24 Compared with Example 1, in Comparative Example 24, tranexamic acid and hydroxyphenylpropionamide benzoic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • Example 25 Compared with Example 1, in Comparative Example 25, diglucosylgallic acid and hydroxyphenylpropanamide benzoic acid were replaced with deionized water, and other conditions were the same as in Example 1.
  • a facial film the formula is shown in Table 1.
  • the preparation method of this mask comprises the steps:
  • component B Pre-dissolve component B at 60-65°C until it is transparent. After component A cools down to 55-60°C, add component B into the water phase pot at a constant speed under stirring conditions. After adding, stir until Evenly dispersed;
  • Example 2 Compared with Application Example 1, in Application Example 2, the composition prepared in Example 1 is replaced by the composition prepared in Example 2, and other conditions are the same as Application Example 1.
  • Application Example 3 replaces the composition prepared in Example 1 with the composition prepared in Example 3, and other conditions are the same as Application Example 1.
  • Example 4 Compared with Application Example 1, in Application Example 4, the composition prepared in Example 1 was replaced with the composition prepared in Example 4, and other conditions were the same as Application Example 1.
  • Step (3) of the preparation method in Application Example 5 the pH of the system was adjusted to 3.5, and other conditions were the same as Application Example 1.
  • Example 1 Compared with Application Example 1, in Comparative Application Examples 1-25, the composition prepared in Example 1 was replaced with the composition prepared in Comparative Example 1-25, and other conditions were the same as Application Example 1.
  • Example 1 Compared with Application Example 1, in Comparative Application Example 26, the composition prepared in Example 1 was replaced with deionized water, and other conditions were the same as Application Example 1.
  • compositions with different concentrations on tyrosinase activity were tested, so as to check the whitening effect of the composition of the present invention.
  • the mass concentrations of the compositions prepared in Examples 1-4 and Comparative Examples 1-25 were respectively diluted to three gradients of 10%, 1%, and 0.1%.
  • In vitro DOPA oxidation reaction method was used to digest human epidermal melanocytes in the logarithmic growth phase with trypsin/EDTA solution, terminate them with trypsin neutralizing solution, and dilute the melanocytes to 1 with MelM medium after centrifugation. ⁇ 10 5 cells/mL, inoculate 100 ⁇ L/well of the diluted liquid in a 96-well plate, and the seeding density is 10 4 cells/well. Overnight, after the cells adhered to the wall, the culture solution was sucked off, and three gradient composition solutions were added to the 96-well plate, 100 ⁇ L per well, and three replicate wells were set up for each concentration.
  • a positive control group containing arbutin (melanocyte + melanocyte culture medium + arbutin 1%, 100 ⁇ L), a negative control group (melanocyte + melanocyte medium) and a blank control group (simply melanocyte prime cell culture medium), and three replicate wells were set up in each group. Place the 24-well plate in an incubator containing 5% CO2 at 37°C for 72 hours.
  • Relative tyrosinase activity [(average absorbance value of drug group-average absorbance value of blank group)/(average absorbance value of negative control group-average absorbance value of blank group)] ⁇ 100%.
  • Comparative example 8 38.73 15.65 2.87 Comparative example 9 58.53 35.64 21.15 Comparative example 10 20.53 15.64 1.15 Comparative example 11 65.86 39.35 10.88 Comparative example 12 53.49 37.87 7.45 Comparative example 13 48.61 32.29 5.10 Comparative example 14 27.15 15.45 3.09 Comparative example 15 25.13 16.53 3.12 Comparative example 16 75.89 44.67 13.54 Comparative example 17 52.61 33.46 12.08 Comparative example 18 52.44 33.21 11.57 Comparative example 19 49.15 40.13 8.82 Comparative example 20 45.62 36.81 6.04 Comparative example 21 39.47 27.65 4.53 Comparative example 22 35.38 21.49 3.62 Comparative example 23 24.05 8.72 0.78 Comparative example 24 30.26 18.37 2.65 Comparative example 25 18.11 6.35 0.96 positive control group 31.44 31.44 31.44 negative control group 100 100 100 100 100 100
  • composition of the present invention combines ⁇ -hydroxy acid, resorcinol derivatives, ascorbic acid and derivatives thereof, tranexamic acid and
  • the combination of gallic acid and its derivatives has a synergistic effect, and has a significant inhibitory effect on human epidermal melanocyte tyrosinase, which is superior to other combinations.
  • Stimulus scoring rules 5-point system. 0 points—no irritation; ⁇ 1 point—slight irritation; ⁇ 2 points—moderately mild irritation, tolerable; ⁇ 3 points—moderate irritation; ⁇ 4 points—moderately severe irritation; ⁇ 5 points—severe irritation Excited.
  • Comparative application example 9 0 no stimulation Comparative application example 10 0 no stimulation Comparative application example 11 0 no stimulation Comparative application example 12 0 no stimulation Comparative application example 13 0 no stimulation Comparative application example 14 0 no stimulation Comparative application example 15 2 mild irritation Comparative application example 16 0 no stimulation Comparative application example 17 0 no stimulation Comparative Application Example 18 0 no stimulation Comparative application example 19 1.5 mild irritation Comparative application example 20 0 no stimulation Comparative application example 21 0 no stimulation Comparative application example 22 2 no stimulation Comparative application example 23 0 no stimulation Comparative application example 24 2 mild irritation Comparative application example 25 1.5 mild irritation Comparative application example 26 0 no stimulation
  • hydroxyphenylpropanamide benzoic acid has a very obvious effect on alleviating the irritation of the product.
  • Application example 4 and comparative application examples 15, 19, 22, 24, and 25 do not contain hydroxyphenylpropanol Aminobenzoic acid component, the product has a certain degree of irritation, indicating that although hydroxyphenylpropanamide benzoic acid has no obvious effect of inhibiting tyrosinase, it is an effective skin anti-sensitivity agent, which can improve skin tolerance. It is an indispensable ingredient in the composition of the present invention. Subsequent experiments will exclude protocols without hydroxyphenylpropanamide.
  • the pH range of the system also has a certain impact on the mildness of the product.
  • the pH value of the system is less than 4, the product has a slight irritation.
  • Increase rate (%) (the disappearance time of the control group - the disappearance time of the experimental group) / the disappearance time of the control group ⁇ 100%
  • Select 120 subjects conduct a random half-face test, use the sample once a night, on D7 (the 7th day) and D28 (the 28th day), under the conditions of temperature 20 ⁇ 2°C and humidity 50 ⁇ 10%, Measure the brightness (L) of the skin color of the subject 20 minutes after the subject's face is cleaned, so as to determine the application examples 1-8 (removal of application example 4) and comparative application examples 1-26 (removal of comparative application examples 15 and 19). , 22, 24, 25) products have the effect of whitening and brightening the skin.
  • Comparative application example 16 59.36 59.49 59.57 0.22% 0.35% Comparative application example 17 59.27 59.46 59.51 0.32% 0.40% Comparative Application Example 18 59.31 59.48 59.59 0.29% 0.47% Comparative application example 20 59.4 59.63 59.86 0.39% 0.77% Comparative application example 21 59.22 59.67 59.8 0.76% 0.98% Comparative application example 23 59.14 59.52 59.66 0.64% 0.88% Comparative application example 26 59.33 59.36 59.35 0.05% 0.03%
  • composition of the present invention combines ⁇ -hydroxy acid, resorcinol derivatives, ascorbic acid and derivatives thereof, tranexamic acid and gallic acid Compounding with its derivatives has a synergistic effect, and has a significant promoting effect on skin whitening and brightening, which is superior to other combinations.
  • the pH of the composition and the pH of the cosmetics containing the composition of the present invention are preferably set at 4-4.5 to maximize its whitening effect.
  • the in vivo test results of the composition of the present invention are consistent with the in vitro test results, which proves that the composition of the present invention has a good whitening effect.

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Abstract

一种具有美白功效的组合物及其制备方法和应用。该组合物包括如下组分：α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物。通过各组分相辅相成，协同增效，从三个维度作用于肌肤，实现快速、有效、持久美白。

Description

一种具有美白功效的组合物及其制备方法和应用 技术领域
本发明属于化妆品技术领域，特别涉及一种具有美白功效的组合物及其制备方法和应用。
背景技术
目前，市售的美白产品存在易引起皮肤敏感刺痛、起效时间长、功效不明显等问题，更有甚者还会引起皮肤炎症甚至对健康造成伤害。因此，美白产品的研发越来越受到皮肤科医师和化妆品企业的重视，如何能开发出安全、温和、疗效好的美白产品是日化品牌及皮肤科亟待解决的问题。
市面上的美白产品美白功效单一，只针对了黑色素产生的部分过程起效，美白效果偏弱，同时，为了追求美白产品的温和性，更多的化妆品企业考虑使用植物类成分代替合成美白剂，但这种方式不仅不能确保产品的安全性而且还降低了产品的有效性。
现有相关技术公开了一种美白淡斑组合物及其应用，所述美白淡斑组合物包括以下原料：蛋黄油、乳木果油、紫檀芪、维生素E、水解神经酰胺III、橙皮提取物、酵母提取物、欧百里香提取物、白柳树皮提取物、毛蕊花提取物、海百合神经活性美白因子、黄芩提取物、氧化白藜芦醇、乳酸杆菌发酵溶胞产物、凝血酸、VC乙基醚、水溶性富勒烯、4-丁基间苯二酚和依克多因。此发明在一定程度上抑制了黑色素的产生，但美白效果并不明显。
现有相关技术公开了一种亮肤美白中药组合物、亮肤美白中药制剂、亮肤美白面膜、制备方法。该中药组合物由以下重量份数的原料组成：连翘果提取物2-4份、防风提取物3-5份、红花提取物2-4份、甘草根提取物3-5份、当归提取物2-4份、丹参提取物2-4份、紫草根提取物2-4份、白芨提取物2-4份、桃仁提取物3-5份、银杏提取物3-5份、水溶性珍珠粉1-3份。该中药组方有活血化瘀，充盈气血的功效，能使人面色红润，淡化暗沉，增强光泽，但美白和淡化色斑的效果较弱。
发明内容
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此，本发明提出一种具有美白功效的组合物及其制备方法和应用，该具有美白功效的组合物温和、安全，能达到快速美白的效果。
本发明的第一方面提供一种具有美白功效的组合物，该组合物包括如下组分：α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物。
本发明所述具有美白功效的组合物的各组分功效如下：
α-羟基酸是指一系列α位有羟基的羧酸的统称，俗称果酸，α-羟基酸可剥离老化的角质层，促进表皮黑色素代谢降解，改善皮肤暗沉、色素过度沉着，使肌肤美白。
没食子酸是强效的酪氨酸酶抑制剂和极佳的抗氧化剂，能有效抑制黑色素转移，达到美白效果， 同时，没食子酸还能预防DNA损伤和抑制皮肤炎症。
间苯二酚衍生物具有超强的抑制酪氨酸酶活性，从而抑制黑色素合成，是一类非常有效的皮肤美白剂，其在很低的浓度也可起效，其中苯乙基间苯二酚是间苯二酚衍生物中有报道的活性最高的酪氨酸酶抑制剂之一。
抗坏血酸及其衍生物是安全有效的皮肤美白剂，抗坏血酸及其衍生物参与体内酪氨酸酶的代谢，促进酪氨酸酶在体内氧化分解，减少酪氨酸转化为黑色素。抗坏血酸及其衍生物还具有潜在的抗炎活性，可以促进伤口愈合和预防炎症后的色素沉积过度。其中抗坏血酸乙基醚是抗坏血酸迄今最好的衍生物，不仅结构稳定还可透皮吸收，生物利用度高。
凝血酸是通过干扰纤溶酶元的结构，并阻止纤溶酶元与角质形成细胞的赖氨酸位点的结合来防止紫外线引起的色素沉着，从而达到淡化色斑效果。凝血酸安全性高、不良反应少，疗效好，对黄褐斑有较好的治疗效果。
本发明申请人在长期生产研究过程中，深入挖掘化妆品原料中具有提亮美白的有效种类，同时根据原料本身的性质和人体皮肤生理特点，通过将上述α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物进行合理复配，从三个维度作用于肌肤：
1)增强代谢：α-羟基酸增强肌肤代谢，促进表皮黑色素代谢降解，即刻提升肌肤的光泽度和柔软度，并促进其他成分的吸收；
2)持续阻断：没食子酸及其衍生物能有效抑制黑色素转移(角化细胞中半乳糖接收器配体，参与将黑色素从黑色素细胞转移到角化细胞的进程)，达到美白效果；
3)抑制生成：通过间苯二酚衍生物抑制酪氨酸酶活性，抗坏血酸及其衍生物促进酪氨酸酶氧化分解和凝血酸干扰纤溶酶活性等三个途径抑制了黑色素的合成，达到美白效果。
本发明制备的组合物具有快速、有效、持久的美白效果。
优选地，所述组合物还包括抗敏剂、多元醇和去离子水，各组分的重量份数如下：α-羟基酸0.1-10份、间苯二酚衍生物0.01-1份、抗坏血酸及其衍生物0.1-10份、凝血酸0.1-10份、没食子酸及其衍生物0.01-1份、抗敏剂0.01-0.1份、多元醇5-10份、去离子水60-90份。
优选地，各组分的重量份数如下α-羟基酸1-10份、间苯二酚衍生物0.01-0.5份、维生素C及其衍生物0.1-10份、凝血酸0.1-10份、没食子酸及其衍生物0.05-1份、抗敏剂0.01-0.1份、多元醇5-10份、去离子水60-90份。
优选地，各组分的重量份数如下α-羟基酸1-10份、间苯二酚衍生物0.01-0.5份、维生素C及其衍生物5-10份、凝血酸0.1-10份、没食子酸及其衍生物0.05-1份、抗敏剂0.01-0.1份、抗敏剂0.01-0.1份、多元醇5-10份、去离子水60-90份。
优选地，各组分的重量份数如下α-羟基酸1-10份、间苯二酚衍生物0.01-0.5份、维生素C及其 衍生物5-10份、凝血酸0.1-5份、没食子酸及其衍生物0.1-0.5份、抗敏剂0.01-0.1份、抗敏剂0.01-0.1份、多元醇5-10份、去离子水60-90份。
优选地，所述α-羟基酸包括乳酸、羟基乙酸、柠檬酸、苹果酸、酒石酸、杏仁酸中的至少一种。更优选地，所述α-羟基酸为乳酸、羟基乙酸、柠檬酸、苹果酸、酒石酸和杏仁酸的混合物。最优选地，所述α-羟基酸为乳酸、羟基乙酸、柠檬酸、苹果酸、酒石酸和杏仁酸按照质量比为1：(0.5-1.5)：(0.1-0.5)：(0.01-0.1)：(0.01-0.1)：(0.01-0.1)混合的混合物。
优选地，所述间苯二酚衍生物包括4-丁基间苯二酚、己基间苯二酚、苯乙基间苯二酚、二甲氧基甲苯基-4-丙基间苯二酚中的至少一种。
优选地，所述抗坏血酸及其衍生物包括抗坏血酸、抗坏血酸磷酸酯钠、抗坏血酸磷酸酯镁、抗坏血酸葡糖苷、抗坏血酸乙基醚中的至少一种。
优选地，所述没食子酸及其衍生物包括二葡糖基棓酸、棓酸、棓酸丙酯、棓酸乙基己酯、鞣花酸中的至少一种。
优选地，所述抗敏剂包括羟苯基丙酰胺苯甲酸、羟基积雪草甙、丹皮酚、β-葡聚糖中的至少一种。
羟苯基丙酰胺苯甲酸是化妆品中有效的止痒抗敏剂，可以发挥抗组胺、抗氧化、抗刺激、抗炎、改善红斑等多重功效，在缓解敏感性肌肤的瘙痒、刺激、泛红上有良好的效果。本发明组合物中加入羟苯基丙酰胺苯甲酸使组合物更安全温和，避免刺激。
羟基积雪草甙是积雪草中含有的三萜皂苷成分，具有抗氧化、抗菌、调节免疫等功能，可以增加皮肤表皮的抵抗力，具有抗发炎、镇静、解毒、消肿的效果，赋予肌肤弹性，强化肌肤的柔软度，可以延缓老化。
丹皮酚具有抗炎作用，对于多种皮肤疾患都有防治作用。
β-葡聚糖具有显著的抗炎、抗过敏活性，能减少皮肤过敏和炎症。
本发明通过额外添加抗敏成分，能够有效抑制组合物可能造成的应激反应，使产品更安全温和。
优选地，所述多元醇为1，3-丙二醇、甘油、1，2-戊二醇、1，2-己二醇中的至少一种。
本发明的第二方面提供所述具有美白功效的组合物的制备方法，包括如下步骤：
将各组分进行混合，得到所述具有美白功效的组合物。
优选地，所述具有美白功效的组合物的制备方法，包括如下步骤：
(1)将间苯二酚衍生物、没食子酸及其衍生物加入多元醇中，加热至50-80℃，搅拌至完全溶解，得到混合液A；
(2)将α-羟基酸、抗坏血酸及其衍生物、凝血酸加入去离子水中，搅拌至完全溶解，得到混合液B；
(3)将混合液A和混合液B进行混合，搅拌至完全均匀，调节pH为4-4.5，得到所述具有美白 功效的组合物。
需要说明的是，在上述制备方法中，抗敏剂的添加需要根据实际选择的物质的溶解性，具体选择在哪个步骤添加，例如选用羟苯基丙酰胺苯甲酸作为抗敏剂，则将羟苯基丙酰胺苯甲酸在步骤(1)中加入多元醇中进行溶解；选用羟基积雪草甙作为抗敏剂，则将羟基积雪草甙在步骤(2)中加入去离子水中进行溶解。
本发明的第三方面提供所述具有美白功效的组合物在化妆品中的应用。
优选地，一种化妆品，包括本发明所述的具有美白功效的组合物和辅料。
优选地，一种面贴膜，包括本发明所述具有美白功效的组合物和辅料。
优选地，所述辅料包括防腐剂、保湿剂、增稠剂中的至少一种。
相对于现有技术，本发明的有益效果如下：
本发明具有美白功效的组合物，将α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物复配使用，通过各组分相辅相成，协同增效，从三个维度作用于肌肤，实现快速、有效、持久美白。
具体实施方式
为了让本领域技术人员更加清楚明白本发明所述技术方案，现列举以下实施例进行说明。需要指出的是，以下实施例对本发明要求的保护范围不构成限制作用。
以下实施例中所用的原料、试剂或装置如无特殊说明，均可从常规商业途径得到，或者可以通过现有已知方法得到。
实施例1
一种具有美白功效的组合物，包括如下重量份数的组分：α-羟基酸5份、苯乙基间苯二酚0.2份、抗坏血酸乙基醚5份、凝血酸5份、二葡糖基棓酸0.3份、羟苯基丙酰胺苯甲酸0.03份、1，2-戊二醇5份、去离子水79.47份。
其中，α-羟基酸为乳酸、羟基乙酸、柠檬酸、苹果酸、酒石酸和杏仁酸按照质量比为1：1：0.3：0.05：0.05：0.05进行混合的混合物。
本实施例具有美白功效的组合物的制备方法，包括如下步骤：
(1)将苯乙基间苯二酚、二葡糖基棓酸和羟苯基丙酰胺苯甲酸加入1，2-戊二醇中，加热至50-80℃，搅拌至完全溶解，得到混合液A；
(2)将α-羟基酸、抗坏血酸乙基醚和凝血酸加入去离子水中，搅拌至完全溶解，得到混合液B；
(3)将混合液A和混合液B进行混合，搅拌至完全均匀，调节pH为4-4.5，得到所述具有美白功效的组合物。
实施例2
一种具有美白功效的组合物，包括如下重量份数的组分：α-羟基酸2份、己基间苯二酚0.5份、抗坏血酸磷酸酯钠1份、凝血酸3份、鞣花酸0.3份、羟基积雪草甙0.05份、甘油10份、去离子水83.15份。
其中，α-羟基酸为柠檬酸、苹果酸、酒石酸和杏仁酸按照质量比为0.3：0.05：0.05：0.05进行混合的混合物。
本实施例具有美白功效的组合物的制备方法，包括如下步骤：
(1)将己基间苯二酚和鞣花酸加入甘油中，加热至50-80℃，搅拌至完全溶解，得到混合液A；
(2)将α-羟基酸、抗坏血酸磷酸酯钠、凝血酸和羟基积雪草甙加入去离子水中，搅拌至完全溶解，得到混合液B；
(3)将混合液A和混合液B进行混合，搅拌至完全均匀，调节pH为4-4.5，得到所述具有美白功效的组合物。
实施例3
一种具有美白功效的组合物，包括如下重量份数的组分：α-羟基酸10份、4-丁基间苯二酚0.1份、抗坏血酸葡糖苷1份、凝血酸1份、棓酸丙酯0.5份、丹皮酚0.02份、1，3-丙二醇5份、去离子水82.38份。
其中，α-羟基酸为乳酸、羟基乙酸、柠檬酸、苹果酸和杏仁酸按照质量比为1：1：0.3：0.05：0.05进行混合的混合物。
本实施例具有美白功效的组合物的制备方法，包括如下步骤：
(1)将4-丁基间苯二酚、棓酸丙酯和丹皮酚加入1，3-丙二醇中，加热至50-80℃，搅拌至完全溶解，得到混合液A；
(2)将α-羟基酸、抗坏血酸葡糖苷和凝血酸加入去离子水中，搅拌至完全溶解，得到混合液B；
(3)将混合液A和混合液B进行混合，搅拌至完全均匀，调节pH为4-4.5，得到所述具有美白功效的组合物。
实施例4
一种具有美白功效的组合物，包括如下重量份数的组分：α-羟基酸5份、苯乙基间苯二酚0.2份、抗坏血酸乙基醚5份、凝血酸5份、二葡糖基棓酸0.3份、1，2-戊二醇5份、去离子水79.5份。
其中，α-羟基酸为乳酸、羟基乙酸按照质量比为1：1进行混合的混合物。
本实施例具有美白功效的组合物的制备方法，包括如下步骤：
(1)将苯乙基间苯二酚和二葡糖基棓酸加入1，2-戊二醇中，加热至50-80℃，搅拌至完全溶解，得到混合液A；
(2)将α-羟基酸、抗坏血酸乙基醚和凝血酸加入去离子水中，搅拌至完全溶解，得到混合液B；
(3)将混合液A和混合液B进行混合，搅拌至完全均匀，调节pH为4-4.5，得到所述具有美白功效的组合物。
对比例1
与实施例1相比，对比例1中将苯乙基间苯二酚、抗坏血酸乙基醚、凝血酸和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例2
与实施例1相比，对比例2中将α-羟基酸替换为去离子水，其他条件与实施例1相同。
对比例3
与实施例1相比，对比例3中将α-羟基酸、抗坏血酸乙基醚、凝血酸和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例4
与实施例1相比，对比例4中将苯乙基间苯二酚替换为去离子水，其他条件与实施例1相同。
对比例5
与实施例1相比，对比例5中将α-羟基酸、苯乙基间苯二酚、凝血酸和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例6
与实施例1相比，对比例6中将抗坏血酸乙基醚替换为去离子水，其他条件与实施例1相同。
对比例7
与实施例1相比，对比例7中将α-羟基酸、苯乙基间苯二酚、抗坏血酸乙基醚和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例8
与实施例1相比，对比例8中将凝血酸替换为去离子水，其他条件与实施例1相同。
对比例9
与实施例1相比，对比例9中将α-羟基酸、苯乙基间苯二酚、抗坏血酸乙基醚和凝血酸替换为去离子水，其他条件与实施例1相同。
对比例10
与实施例1相比，对比例10中将二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例11
与实施例1相比，对比例11中将α-羟基酸和苯乙基间苯二酚替换为去离子水，其他条件与实施例1相同。
对比例12
与实施例1相比，对比例12中将α-羟基酸和抗坏血酸乙基醚替换为去离子水，其他条件与实施例1相同。
对比例13
与实施例1相比，对比例13中将α-羟基酸和凝血酸替换为去离子水，其他条件与实施例1相同。
对比例14
与实施例1相比，对比例14中将α-羟基酸和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例15
与实施例1相比，对比例15中将α-羟基酸和羟苯基丙酰胺苯甲酸替换为去离子水，其他条件与实施例1相同。
对比例16
与实施例1相比，对比例16中将苯乙基间苯二酚和抗坏血酸乙基醚替换为去离子水，其他条件与实施例1相同。
对比例17
与实施例1相比，对比例17中将苯乙基间苯二酚和凝血酸替换为去离子水，其他条件与实施例1相同。
对比例18
与实施例1相比，对比例18中将苯乙基间苯二酚和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例19
与实施例1相比，对比例19中将苯乙基间苯二酚和羟苯基丙酰胺苯甲酸替换为去离子水，其他条件与实施例1相同。
对比例20
与实施例1相比，对比例20中将抗坏血酸乙基醚和凝血酸替换为去离子水，其他条件与实施例1相同。
对比例21
与实施例1相比，对比例21中将抗坏血酸乙基醚和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例22
与实施例1相比，对比例22中将抗坏血酸乙基醚和羟苯基丙酰胺苯甲酸替换为去离子水，其他条件与实施例1相同。
对比例23
与实施例1相比，对比例23中将凝血酸和二葡糖基棓酸替换为去离子水，其他条件与实施例1相同。
对比例24
与实施例1相比，对比例24中将凝血酸和羟苯基丙酰胺苯甲酸替换为去离子水，其他条件与实施例1相同。
对比例25
与实施例1相比，对比例25中将二葡糖基棓酸和羟苯基丙酰胺苯甲酸替换为去离子水，其他条件与实施例1相同。
应用例1
一种面贴膜，配方见表1所示。
表1
Figure PCTCN2021132449-appb-000001
该面贴膜的制备方法，包括如下步骤：
(1)将A组分投入到水相锅，80-85℃下搅拌至完全溶解，降温；
(2)将B组分在60-65℃预先溶解至透明，待A组分降温至55-60℃，在搅拌条件下将B组分匀速加入到水相锅中，加入完毕后，搅拌至分散均匀；
(3)降温至40℃以下，再加入C相，搅拌至分散均匀，调整体系的pH为4-4.5；
(4)检验合格后，200目过滤出料即可。
应用例2
与应用例1相比，应用例2中将实施例1制备的组合物替换为实施例2制备的组合物，其他条件 与应用例1相同。
应用例3
与应用例1相比，应用例3将实施例1制备的组合物替换为实施例3制备的组合物，其他条件与应用例1相同。
应用例4
与应用例1相比，应用例4中将实施例1制备的组合物替换为实施例4制备的组合物，其他条件与应用例1相同。
应用例5
与应用例1相比，应用例5中制备方法的步骤(3)中，调整体系的pH为3.5，其他条件与应用例1相同。
应用例6
与应用例1相比，应用例6中制备方法的步骤(3)中，调整体系的pH为5，其他条件与应用例1相同。
应用例7
与应用例1相比，应用例7中制备方法的步骤(3)中，调整体系的pH为5.5，其他条件与应用例1相同。
应用例8
与应用例1相比，应用例8中制备方法的步骤(3)中，调整体系的pH为6，其他条件与应用例1相同。
对比应用例1-25
与应用例1相比，对比应用例1-25中分别将实施例1制备的组合物替换为对比例1-25制备的组合物，其他条件与应用例1相同。
对比应用例26
与应用例1相比，对比应用例26中将实施例1制备的组合物替换为去离子水，其他条件与应用例1相同。
试验例1体外美白测试
1.1实验目的
以护肤品中常用美白成分熊果苷对比，测试不同浓度的组合物对酪氨酸酶活性的抑制效果，从而检查本发明组合物的美白作用。
1.2参照品制备
配制质量浓度为1％的熊果苷溶液。
分别将实施例1-4和对比例1-25制备的组合物的质量浓度稀释为10％、1％、0.1％三个梯度。
1.3实验方法
采用体外氧化DOPA反应法，用胰蛋白酶/EDTA溶液消化处于对数生长期的人表皮黑素细胞，用胰蛋白酶中和液对其进行终止，离心后用MelM培养基将黑素细胞稀释成1×10 5个/mL，取稀释后液体接种于96孔板100μL/孔，接种密度为10 4个/孔。过夜，待细胞贴壁，吸去培养液，并向96孔板中分别加入3个梯度组合物溶液，每孔100μL，每个浓度均设立3个复孔。设立含熊果苷的阳性对照组(黑素细胞+黑素细胞培养基+熊果苷1％、100μL)、阴性对照组(黑素细胞+黑素细胞培养基)和空白对照组(单纯黑素细胞培养基)，每组设立3个复孔。将24孔板放置于37℃、含5％CO 2的孵箱中培养72h，药物处理结束后，弃上清液用PBS液清洗黑素细胞2-3遍，分别于每孔中加入100μL含1％TritonX-100(用PBS液配制)，于振荡器上低速震荡30min，将96孔板放置于-20℃冰箱中1h，取出后于室温下使其融化，是黑素色完全裂解。每孔加入100μL浓度为0.1％L-DOPA(PBS液配制)溶液，继续于37℃孵育2h，酶标仪测定标本吸光度值，酶标仪测定波长为490nm。
酪氨酸酶相对活性＝[(药物组平均吸光值-空白组平均吸光值)/(阴性对照组平均吸光值-空白组平均吸光值)]×100％。
1.4实验结果
结果见表2所示。
表2
样品组 组合物0.1％ 组合物1％ 组合物10％
实施例1 7.66 2.59 0.26
实施例2 10.82 3.15 0.31
实施例3 16.39 5.64 0.69
实施例4 7.70 2.60 0.26
对比例1 99.98 98.51 95.32
对比例2 30.24 13.22 2.85
对比例3 48.88 37.52 13.90
对比例4 54.88 34.52 5.90
对比例5 57.13 38.41 19.51
对比例6 47.13 28.41 4.51
对比例7 68.73 45.65 22.87
对比例8 38.73 15.65 2.87
对比例9 58.53 35.64 21.15
对比例10 20.53 15.64 1.15
对比例11 65.86 39.35 10.88
对比例12 53.49 37.87 7.45
对比例13 48.61 32.29 5.10
对比例14 27.15 15.45 3.09
对比例15 25.13 16.53 3.12
对比例16 75.89 44.67 13.54
对比例17 52.61 33.46 12.08
对比例18 52.44 33.21 11.57
对比例19 49.15 40.13 8.82
对比例20 45.62 36.81 6.04
对比例21 39.47 27.65 4.53
对比例22 35.38 21.49 3.62
对比例23 24.05 8.72 0.78
对比例24 30.26 18.37 2.65
对比例25 18.11 6.35 0.96
阳性对照组 31.44 31.44 31.44
阴性对照组 100 100 100
从表2的数据可以看出，与阴性对照组相比，阳性对照组、实施例1-4和对比例1-25都具有酪氨酸酶活性的抑制效果。由实施例1和实施例4相比可以看出，羟苯基丙酰胺苯甲酸对酪氨酸酶活性基本没有抑制作用，其他成分均有抑制效果；由对比例1、3、5、7、9可以看出，苯乙基间苯二酚的抑制效果最强，抗坏血酸乙基醚的效果次之。实施例1-4的抑制酪氨酸酶活性的效果明显优于对比例1-25，说明本发明组合物将α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物进行复配，具有协同增效效果，对于人表皮黑素细胞酪氨酸酶有显著的抑制效果，优于其他组合方式。
试验例2刺激性测试
2.1实验目的
通过消费者直接使用测试，确认产品的刺激性。
2.2实验方案
选取60名消费者，开始使用时和使用1周后，分别对应用例1-8和对比应用例1-26制备的面贴膜的刺激性评分。
2.3判定标准
刺激性评分规则：5分制。0分—无刺激；≤1分—轻微刺激；≤2分—中轻度剌激，可耐受；≤3分—中度刺激；≤4分—中重度剌激；≤5分—严重剌激。
2.4刺激性测试结果
结果见表3所示。
表3
样品组 评分 刺激程度
应用例1 0 无刺激
应用例2 0 无刺激
应用例3 0 无刺激
应用例4 2.5 中度刺激
应用例5 1 轻微刺激
应用例6 0 无刺激
应用例7 0 无刺激
应用例8 0 无刺激
对比应用例1 0 无刺激
对比应用例2 0 无刺激
对比应用例3 0 无刺激
对比应用例4 0 无刺激
对比应用例5 0 无刺激
对比应用例6 0 无刺激
对比应用例7 0 无刺激
对比应用例8 0 无刺激
对比应用例9 0 无刺激
对比应用例10 0 无刺激
对比应用例11 0 无刺激
对比应用例12 0 无刺激
对比应用例13 0 无刺激
对比应用例14 0 无刺激
对比应用例15 2 中轻度刺激
对比应用例16 0 无刺激
对比应用例17 0 无刺激
对比应用例18 0 无刺激
对比应用例19 1.5 中轻度刺激
对比应用例20 0 无刺激
对比应用例21 0 无刺激
对比应用例22 2 无刺激
对比应用例23 0 无刺激
对比应用例24 2 中轻度刺激
对比应用例25 1.5 中轻度刺激
对比应用例26 0 无刺激
由表3数据可以看出，羟苯基丙酰胺苯甲酸对减缓产品的刺激性具有非常明显的效果，应用例4以及对比应用例15、19、22、24、25由于不含有羟苯基丙酰胺苯甲酸组分，产品均有一定程度的刺激，说明羟苯基丙酰胺苯甲酸虽然没有明显的抑制酪氨酸酶效果，但其是有效的肌肤抗敏剂，能提升肌肤耐受力，是本发明组合物中不可或缺的成分。后续实验将剔除没有羟苯基丙酰胺苯甲酸的方案。
另外，体系的pH值范围对产品的温和性也有一定的影响，如应用例5，当体系的pH值小于4时，产品有轻微的刺激。
试验例3角质更新时间测试
3.1实验目的
本试验通过测试对皮肤的丹磺酰氯染色的消退时间，确认表皮更新时间，以此确认产品促进肌肤新陈代谢的程度。
3.2试验方法
选取60名健康、无皮肤病疾患的志愿者，用丹磺酰氯对受试者左右前臂内侧皮肤进行荧光染色：将纱布剪成1cm 2大小，涂满丹磺酰氯溶液，然后平贴在已选定的受试部位，上覆玻璃红，用胶带固定。24h后除去丹磺酰氯斑贴物，用水洗去过量的染液。以后每天，按盲法专人在紫外灯下(波长300nm-400nm)检测荧光消退情况。
受试者在荧光染色部位，一侧贴敷应用例1-8(剔除应用例4)以及对比应用例1-23(剔除对比应用例15、19、22)作为实验组，另一侧贴敷对比应用例26作为对照组，每天使用1次，每次20min，然后用清水清洗掉。样品涂布过程亦按单盲法由专人操作，并一直到该部位不再有荧光标记为止。
3.3计算方法
增快速率(％)＝(对照组消退时间－实验组消退时间)/对照组消退时间×100％
3.4荧光消退时间分析
结果见表4所示。
表4
Figure PCTCN2021132449-appb-000002
Figure PCTCN2021132449-appb-000003
从表4的数据可以看出，实验组均有一定的促进角质更新的效果。由对比应用例1、3、5、7、9可以看出，组合物中的单独组分以α-羟基酸对促进角质更新的效果最为显著，其次为凝血酸。应用例1对促进角质更新的效果均明显比对比应用例的效果好，说明本发明组合物将α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物进行复配，具有协同增效效果，对角质细胞的脱落有促进效果。
另外，应用例6-8随着体系的pH值增加，产品对促进角质更新的作用效果降低，低于应用例1-3，在pH越接近中性时效果越弱，应用例5在pH为3.5时效果最为明显。
试验例4祛斑美白测试
4.1实验目的
选取120名受试者，随机半脸测试，每晚使用一次样品，于D7(第7天)、D28(第28天)时，在温度20±2℃，湿度50±10％的条件下，在受试者脸部清洁后20min时对脸部肤色亮度(L)进行测量，以此判定应用例1-8(剔除应用例4)以及对比应用例1-26(剔除对比应用例15、19、22、24、25)的产品对皮肤的美白提亮功效。
4.2实验方案
参考方法：《化妆品祛斑美白功效测试方法》2019版。
4.3判定标准
L值有显著差异，L值越大，颜色越偏向白色，L值越小，颜色越偏向黑色。
4.4 L值测试结果分析
结果见表5所示。
表5
样品组 D0 D7 D28 D7变化率 D28变化率
应用例1 59.42 60.06 61.13 1.08％ 2.88％
应用例2 59.51 60.02 61.09 0.86％ 2.66％
应用例3 59.14 59.67 60.62 0.90％ 2.50％
应用例5 59.45 60.47 62.41 1.72％ 4.98％
应用例6 59.27 59.67 60.12 0.67％ 1.43％
应用例7 59.18 59.44 59.78 0.44％ 1.01％
应用例8 59.21 59.36 59.58 0.25％ 0.62％
对比应用例1 59.34 59.36 59.4 0.03％ 0.10％
对比应用例2 59.34 59.74 59.91 0.67％ 0.96％
对比应用例3 59.16 59.22 59.37 0.10％ 0.35％
对比应用例4 59.16 59.45 59.67 0.49％ 0.86％
对比应用例5 59.55 59.60 59.69 0.08％ 0.24％
对比应用例6 59.55 59.94 60.37 0.65％ 1.38％
对比应用例7 59.17 59.20 59.26 0.05％ 0.15％
对比应用例8 59.17 59.62 59.8 0.76％ 1.06％
对比应用例9 59.26 59.30 59.37 0.07％ 0.19％
对比应用例10 59.26 59.74 59.85 0.81％ 1.00％
对比应用例11 59.44 59.64 59.88 0.34％ 0.74％
对比应用例12 59.23 59.61 59.75 0.64％ 0.88％
对比应用例13 59.26 59.57 59.63 0.52％ 0.62％
对比应用例14 59.47 59.71 59.87 0.40％ 0.67％
对比应用例16 59.36 59.49 59.57 0.22％ 0.35％
对比应用例17 59.27 59.46 59.51 0.32％ 0.40％
对比应用例18 59.31 59.48 59.59 0.29％ 0.47％
对比应用例20 59.4 59.63 59.86 0.39％ 0.77％
对比应用例21 59.22 59.67 59.8 0.76％ 0.98％
对比应用例23 59.14 59.52 59.66 0.64％ 0.88％
对比应用例26 59.33 59.36 59.35 0.05％ 0.03％
从表5的数据可以看出，应用例和对比应用例均有一定的皮肤美白提亮功效。由对比例1、3、5、7、9可以看出，组合物中的单独组分以苯乙基间苯二酚对皮肤亮度的影响最大，其次为抗坏血酸乙基醚。应用例1-3和应用例5的效果均明显比对比应用例的效果好，说明本发明组合物将α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物进行复配，具有协同增效效果，对皮肤的美白提亮有显著的促进效果，优于其他组合方式。
另外，应用例6-8随着体系的pH值增加，产品对皮肤的美白提亮的作用效果降低，低于应用例1-3，在pH越接近中性时效果越弱，应用例5在pH为3.5时效果最为明显。出于安全性考虑，本发明将组合物的pH及含有本发明组合物的化妆品的pH优选为4-4.5，以最大发挥其美白效果。
经上述试验测试，本发明组合物的体内测试结果与体外测试结果是吻合的，证明本发明组合物具有很好的美白效果。
以上对本发明的较佳实施方式进行了具体说明，但本发明创造并不限于所述实施例，熟悉本领域的技术人员在不违背本发明精神的前提下还可作出种种的等同变型或替换，这些等同的变型或替换均包含在本申请权利要求所限定的范围内。

Claims (10)

  1. 一种组合物，其特征在于，包括如下组分：α-羟基酸、间苯二酚衍生物、抗坏血酸及其衍生物、凝血酸和没食子酸及其衍生物。
  2. 根据权利要求1所述的组合物，其特征在于，所述组合物还包括抗敏剂、多元醇和水，各组分的重量份数如下：α-羟基酸0.1-10份、间苯二酚衍生物0.01-1份、抗坏血酸及其衍生物0.1-10份、凝血酸0.1-10份、没食子酸及其衍生物0.01-1份、抗敏剂0.01-0.1份、多元醇5-10份、水60-90份。
  3. 根据权利要求1所述的组合物，其特征在于，所述α-羟基酸包括乳酸、羟基乙酸、柠檬酸、苹果酸、酒石酸、杏仁酸中的至少一种。
  4. 根据权利要求1所述的组合物，其特征在于，所述间苯二酚衍生物包括4-丁基间苯二酚、己基间苯二酚、苯乙基间苯二酚、二甲氧基甲苯基-4-丙基间苯二酚中的至少一种。
  5. 根据权利要求1所述的组合物，其特征在于，所述抗坏血酸及其衍生物包括抗坏血酸、抗坏血酸磷酸酯钠、抗坏血酸磷酸酯镁、抗坏血酸葡糖苷、抗坏血酸乙基醚中的至少一种；所述没食子酸及其衍生物包括二葡糖基棓酸、棓酸、棓酸丙酯、棓酸乙基己酯、鞣花酸中的至少一种。
  6. 根据权利要求2所述的组合物，其特征在于，所述抗敏剂包括羟苯基丙酰胺苯甲酸、羟基积雪草甙、丹皮酚、β-葡聚糖中的至少一种。
  7. 权利要求1-6任一项所述的组合物的制备方法，其特征在于，包括以下步骤：
    将各组分进行混合，得到所述组合物。
  8. 权利要求1-6任一项所述的组合物在化妆品中的应用。
  9. 一种化妆品，其特征在于，包括权利要求1-6任一项所述的组合物和辅料。
  10. 一种面贴膜，其特征在于，包括权利要求1-6任一项所述的组合物和辅料。
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