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CN-121971319-A - Hair-loss-preventing and hair-care shampoo and preparation method thereof

CN121971319ACN 121971319 ACN121971319 ACN 121971319ACN-121971319-A

Abstract

The invention relates to the technical field of shampoos, in particular to an anti-hair-loss hair-care shampoo and a preparation method thereof, wherein the anti-hair-loss hair-care shampoo comprises sodium laureth sulfate, cocamidopropyl betaine, polysorbate 80, adenosine, mercapto polyethylene glycol modified beta-cyclodextrin, selenized maleimide modified polyvinyl alcohol, propyl gallate, sodium chloride, phenoxyethanol, citric acid and essence; according to the invention, the problem that the adenosine is continuously destroyed by the hydroperoxide generated by the automatic oxidation of polysorbate 80 in the existing anti-hair-loss shampoo formula is effectively solved by three components of sulfhydryl polyethylene glycol modified beta-cyclodextrin, selenized maleimide modified polyvinyl alcohol and propyl gallate.

Inventors

  • FANG YUXIONG
  • MENG YI
  • ZHANG HENGRUI
  • CHENG LINYOU

Assignees

  • 广西花之丽人化妆品有限公司

Dates

Publication Date
20260505
Application Date
20260330

Claims (8)

  1. 1. The hair-loss-preventing and hair-care shampoo is characterized by comprising, by weight, 12-18 parts of sodium laureth sulfate, 3-6 parts of cocamidopropyl betaine, 80-3 parts of polysorbate, 0.1-0.5 part of adenosine, 0.8-1.5 part of mercapto polyethylene glycol modified beta-cyclodextrin, 0.3-0.8 part of selenized maleimide modified polyvinyl alcohol, 0.05-0.20 part of propyl gallate, 0.5-2.0 parts of sodium chloride, 0.5-1.0 part of phenoxyethanol, 0.1-0.3 part of citric acid and 0.1-0.5 part of essence, and adding deionized water to make up the balance to 100 parts.
  2. 2. The hair-loss preventing and caring shampoo according to claim 1, wherein the preparation method of the sulfhydryl polyethylene glycol modified beta-cyclodextrin comprises the following steps: S11, dissolving beta-cyclodextrin in distilled water, placing in an ice bath for cooling to 0-5 ℃, adding a sodium hydroxide aqueous solution for stirring uniformly, dropwise adding an acetone solution of p-toluenesulfonyl chloride, maintaining the reaction temperature at 0-5 ℃, adjusting the pH value to 8.5 after the reaction is finished, standing at 4 ℃ overnight to precipitate, filtering, washing, recrystallizing, and drying in vacuum to obtain an intermediate A1; s12, dissolving the intermediate A1 in anhydrous N, N-dimethylformamide, adding sodium azide, reacting for 24 hours under the protection of 80 ℃ nitrogen, cooling, pouring into acetone for precipitation, filtering, washing and drying in vacuum to obtain an intermediate A2; s13, dissolving the intermediate A2 in distilled water, adding triphenylphosphine, stirring at room temperature for reaction for 12 hours, dialyzing for 72 hours by a dialysis bag with a molecular weight cut-off of 1000 Da to remove by-product triphenylphosphine oxide, and freeze-drying to obtain an intermediate A3; S14, dissolving the intermediate A3 in 0.1mol/L of pH8.5 borate buffer solution, adding N-hydroxysuccinimide ester-polyethylene glycol-o-pyridine disulfide, reacting for 4 hours at room temperature, dialyzing for 72 hours by using a dialysis bag with the molecular weight cutoff of 3500 Da, and freeze-drying to obtain an intermediate A4; S15, dissolving the intermediate A4 in a degassed phosphate buffer with the pH value of 8.0, adding dithiothreitol, reacting for 1 hour under the protection of nitrogen at room temperature, dialyzing for 48 hours by using degassed distilled water containing 1 mmol/L ethylene diamine tetraacetic acid disodium salt, and freeze-drying to obtain the sulfhydryl polyethylene glycol modified beta-cyclodextrin.
  3. 3. The hair loss preventing and caring shampoo according to claim 1, wherein the preparation method of the selenized maleimide modified polyvinyl alcohol comprises the following steps: S21, dissolving maleic anhydride in glacial acetic acid, stirring and dissolving at 50 ℃, adding glycine, stirring and reacting for 2 hours, adding sodium acetate and acetic anhydride, heating to 110 ℃ and reacting for 6 hours, cooling, pouring into ice water, extracting with ethyl acetate, drying and evaporating, and recrystallizing with absolute ethyl alcohol to obtain an intermediate B1; s22, dissolving polyvinyl alcohol in anhydrous dimethyl sulfoxide to obtain a polyvinyl alcohol solution, pre-activating an intermediate B1 by using N, N' -dicyclohexylcarbodiimide and 4-dimethylaminopyridine in an ice bath for 30 minutes, slowly dropwise adding the polyvinyl alcohol solution, stirring at room temperature for reacting for 48 hours, filtering, pouring filtrate into anhydrous diethyl ether for precipitation, collecting the precipitate, dialyzing for 48 hours by using 4 ℃ distilled water, and freeze-drying to obtain an intermediate B2; S23, dissolving the intermediate B2 in a mixed solvent of dimethyl sulfoxide and degassed distilled water, introducing nitrogen for protection, adding selenious acid and catalytic amount of p-toluenesulfonic acid, stirring and reacting for 24 hours under the protection of 60 ℃ nitrogen, cooling, dialyzing for 48 hours by using the degassed distilled water containing 1 mmol/L ethylene diamine tetraacetic acid disodium salt, and freeze-drying to obtain the selenized maleimide modified polyvinyl alcohol.
  4. 4. The hair-protecting shampoo according to claim 3, wherein the volume ratio of dimethyl sulfoxide to degassed distilled water in the mixed solvent of dimethyl sulfoxide and degassed distilled water is 4:1.
  5. 5. The hair-protecting shampoo according to claim 1, wherein the sulfhydryl polyethylene glycol modified beta-cyclodextrin and the selenized maleimide modified polyvinyl alcohol are mixed in a phosphate buffer solution of 0.1mol/L before being added into the shampoo formulation, and are pre-crosslinked for 4 hours under the protection of nitrogen at room temperature to form a pre-crosslinked compound, and then the pre-crosslinked compound is added into the shampoo formulation.
  6. 6. The hair-loss prevention and hair-care shampoo according to claim 5, wherein the phosphate buffer solution with the concentration of 0.1mol/L contains 1mmol/L disodium ethylenediamine tetraacetate, the pH is 6.5-7.0, and the hair-loss prevention and hair-care shampoo is subjected to degassing treatment in advance.
  7. 7. The method for preparing the hair-loss preventing and protecting shampoo according to any one of claims 1 to 6, which is characterized by comprising the following steps: S1, preparing a surfactant matrix solution, namely heating deionized water to 70-75 ℃, adding sodium laureth sulfate and cocamidopropyl betaine, stirring until the sodium laureth sulfate and the cocamidopropyl betaine are completely dissolved, and cooling to below 40 ℃ to obtain the surfactant matrix solution; S2, preparing an adenosine solubilizing solution, namely dissolving adenosine in a small amount of hot deionized water, adding polysorbate 80, stirring until the mixture is uniform and transparent, cooling, adding the mixture into a surfactant matrix solution, and fully and uniformly mixing to obtain an adenosine solubilizing solution; s3, adding the pre-crosslinked compound, namely dissolving propyl gallate in a small amount of ethanol, adding the propyl gallate into an adenosine increasing solution, and uniformly stirring; s4, adjusting the viscosity and the pH, namely adding sodium chloride to adjust the viscosity of the system, adjusting the pH to 4.5-6.0 by using citric acid, adding phenoxyethanol and essence, fully and uniformly stirring, and filtering to obtain the hair-loss-preventing and hair-care shampoo.
  8. 8. The method according to claim 7, wherein the pre-crosslinking compound is added in step S3 at a temperature below 40 ℃ under the protection of nitrogen, and the pre-crosslinking compound is prevented from directly contacting with oxygen in the air.

Description

Hair-loss-preventing and hair-care shampoo and preparation method thereof Technical Field The invention relates to the technical field of shampoos, in particular to an anti-hair-loss and hair-care shampoo and a preparation method thereof. Background Anti-hair loss shampoos are an important product type in the field of hair care, the core of which is to deliver active ingredients to the scalp through daily cleaning processes, improve the hair follicle microenvironment, and delay or reduce the hair loss phenomenon. Adenosine is a well-known anti-hair loss active ingredient, and plays an anti-hair loss role by promoting energy metabolism of hair follicle cells, regulating expression of growth factors and other mechanisms, and has been proved to be effective by a plurality of researches and widely applied to anti-hair loss products. Polysorbate 80 is used as nonionic emulsifier and solubilizer in shampoo formulation containing adenosine, and has the main functions of solubilizing active ingredients with poor water solubility such as adenosine and oil-soluble components such as dissolved essential oil. However, polysorbate 80 contains unsaturated double bonds and polyoxyethylene chains in its molecular structure, and autoxidation occurs during storage (under light irradiation, high temperature, and trace metal ion catalysis), and oxidative species such as hydroperoxides are generated by free radical chain reaction. The hydroperoxide is a strong oxidant, can oxidatively degrade active ingredients sensitive to oxidation, adenine rings in adenosine molecules contain amino groups, ribose parts contain hydroxyl groups, and are easy to attack by oxidizing, so that the content is reduced and the efficacy is reduced. Solutions to such problems in the prior art have focused mainly on the two directions, namely, adding phenolic antioxidants (e.g., BHT, BHA) to the formulation to inhibit the autoxidation chain reaction of polysorbate 80, and on the other hand, using ultra-refined or low peroxide grade polysorbate 80 feedstock to control the initial hydroperoxide content from the source. However, phenolic antioxidants have limited solubility, uneven distribution and stability problems in water-based shampoo systems, and low peroxide value materials can only control the initial state and cannot prevent the continuous autoxidation process of the formulation throughout shelf life (typically 3 years). Disclosure of Invention (1) Technical problem to be solved The invention aims to provide an anti-hair-loss hair-care shampoo and a preparation method thereof, which are used for solving the problem that the anti-hair-loss effect is reduced due to the fact that adenosine is damaged by hydroperoxide generated by polysorbate 80. (2) Technical proposal In order to achieve the aim, on the one hand, the invention provides an anti-hair-loss hair-care shampoo, which comprises, by weight, 12-18 parts of sodium laureth sulfate, 3-6 parts of cocamidopropyl betaine, 1-3 parts of polysorbate, 0.1-0.5 part of adenosine, 0.8-1.5 parts of mercapto polyethylene glycol modified beta-cyclodextrin, 0.3-0.8 part of selenized maleimide modified polyvinyl alcohol, 0.05-0.20 part of propyl gallate, 0.5-2.0 parts of sodium chloride, 0.5-1.0 part of phenoxyethanol, 0.1-0.3 part of citric acid, 0.1-0.5 part of essence, and the balance of deionized water. Further, the preparation method of the sulfhydryl polyethylene glycol modified beta-cyclodextrin comprises the following steps: S11, dissolving beta-cyclodextrin in distilled water, placing in an ice bath for cooling to 0-5 ℃, adding a sodium hydroxide aqueous solution for stirring uniformly, dropwise adding an acetone solution of p-toluenesulfonyl chloride, maintaining the reaction temperature at 0-5 ℃, adjusting the pH value to 8.5 after the reaction is finished, standing at 4 ℃ overnight to precipitate, filtering, washing, recrystallizing, and drying in vacuum to obtain an intermediate A1; s12, dissolving the intermediate A1 in anhydrous N, N-dimethylformamide, adding sodium azide, reacting for 24 hours under the protection of 80 ℃ nitrogen, cooling, pouring into acetone for precipitation, filtering, washing and drying in vacuum to obtain an intermediate A2; s13, dissolving the intermediate A2 in distilled water, adding triphenylphosphine, stirring at room temperature for reaction for 12 hours, dialyzing for 72 hours by a dialysis bag with a molecular weight cut-off of 1000 Da to remove by-product triphenylphosphine oxide, and freeze-drying to obtain an intermediate A3; S14, dissolving the intermediate A3 in 0.1mol/L of pH8.5 borate buffer solution, adding N-hydroxysuccinimide ester-polyethylene glycol-o-pyridine disulfide, reacting for 4 hours at room temperature, dialyzing for 72 hours by using a dialysis bag with the molecular weight cutoff of 3500 Da, and freeze-drying to obtain an intermediate A4; S15, dissolving the intermediate A4 in a degassed phosphate buffer with the pH value of 8.0, adding dit