WO2020077956A1 - 一种含蚕丝蛋白成分的去屑止痒洗发养发组合物及其制备方法 - Google Patents

一种含蚕丝蛋白成分的去屑止痒洗发养发组合物及其制备方法 Download PDF

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WO2020077956A1
WO2020077956A1 PCT/CN2019/080353 CN2019080353W WO2020077956A1 WO 2020077956 A1 WO2020077956 A1 WO 2020077956A1 CN 2019080353 W CN2019080353 W CN 2019080353W WO 2020077956 A1 WO2020077956 A1 WO 2020077956A1
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solution
silk
parts
silkworm
hydrolysate
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PCT/CN2019/080353
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English (en)
French (fr)
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张向阳
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广州骐源生物科技有限公司
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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
    • A61K8/40—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
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/20—Halogens; Compounds 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
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34—Alcohols
    • A61K8/345—Alcohols containing more than one hydroxy group
    • 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
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/42—Amides
    • 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
    • A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
    • 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
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/4946—Imidazoles or their condensed derivatives, e.g. benzimidazoles
    • 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
    • A61K8/63—Steroids; 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/731—Cellulose; Quaternized cellulose derivatives
    • 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
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/006—Antidandruff preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/02—Preparations for cleaning the hair
    • 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

Definitions

  • the invention relates to a shampoo and hair care composition, which belongs to the technical field of chemical care products, in particular to an anti-dandruff and itching shampoo and hair care composition containing silk protein components and a preparation method thereof.
  • Dandruff is a common physiological phenomenon in humans and a repetitive multiple skin problem. Increased dandruff will not only be accompanied by itching of the scalp, but also bring discomfort to people, in particular, full dandruff also greatly affects the appearance. Traditional anti-dandruff and itching theory believes that dandruff is caused by fungi such as Malassezia furfur. The focus of everyone's research is how to use better fungicides to inhibit or kill these microorganisms.
  • anti-dandruff and anti-itch ingredients with bactericidal effect are applied to anti-dandruff and anti-itch shampoo products.
  • synthetic fungicides such as: ganbaosu, ZPT, OTC, etc., or plant fungicides such as honeysuckle, lemongrass, tea tree oil, sophora flavescens, etc., but even so, there is still no product that can better Solve the problem of dandruff and itchy scalp. Because, ignoring another key factor in the formation of the scalp-dry skin caused by dandruff and scalp itching.
  • silk is composed of a layer of sericin on the outside and a layer of silk fibroin on the inside. Whether sericin is sericin or silk fibroin, keratin is a good natural skin care material.
  • silkworm specially developed and cultured for cosmetics, so it brings many problems such as too many raw material impurities and high allergy rate.
  • the object of the present invention is to provide an anti-dandruff antipruritic shampoo and hair care composition containing silk protein components, by using a shampoo containing silk protein components to improve and maintain the scalp
  • a shampoo containing silk protein components to improve and maintain the scalp
  • Another object of the present invention is to provide a method for preparing an anti-dandruff anti-itch shampoo and hair care composition containing the silk protein component.
  • a method for preparing silk protein hydrolysate includes the following steps:
  • the cocoon amount is 0.4-10%
  • the hydrolysis temperature is controlled at 50-100 °C water bath temperature degumming 2-4h, filtered to obtain hydrolyzed silk sericin (Filtrate) and silk fibroin fiber (filter residue); the resulting filtrate is desalted by electrodialysis device, the obtained desalinated silkworm protein is retained for use, and the salt solution removed can be used for the next hydrolysis, thereby reducing emissions, reducing costs, and reducing Pollution;
  • step 1) the method for cultivating silkworm cocoons is:
  • the silkworm is a second-generation silkworm obtained from the sericulture technology station.
  • the silkworm is used to stabilize the content of the sericin and silk fibroin, so as to obtain a stable hydrolysis ratio of hydrolyzed sericin and hydrolyzed silk fibroin. product;
  • the culture environment of silkworm is related to microbial control of later products and silkworm leaf disease; in the present invention, the culture environment of silkworm is aseptic, ventilated, and dry silkworm indoor breeding to reduce pathogens and microorganisms of the final product Other risks;
  • Silk is an active protein and needs to be stored in a cool, dry and ventilated place.
  • the neutral salt solution is selected from anhydrous CaCl 2 , CaCl 2 -H 2 O, CaCl 2 -2H 2 O or LiBr solutions with a mass concentration of 30-50%.
  • step 3 the control of the hydrolysis end point is to ensure that the molecular weight of the silk protein of the final product obtained in step 5) is controlled in the range of 20,000-200,000 Daltons, mainly concentrated in 10
  • the range of 10,000-200,000 Daltons, and the hydrolysate obtained from other patents or processes are silk peptides or amino acids; the control of the molecular weight of the final product is the guarantee of the efficacy of the product obtained by the product of the present invention.
  • an anti-dandruff anti-itch shampoo and hair care composition containing silk protein components includes the following components in weight ratio:
  • the anti-dandruff anti-itch shampoo and hair care composition containing the silk protein component is prepared by the following process:
  • step 2) Filter the solution in step 1) to form degummed hydrolysate and silk fibroin fibers;
  • step 3 The degummed hydrolysate filtered in step 2) is divided into sericin hydrolysate and dialysis ion solution by electrodialysis, and the sericin hydrolysate is retained.
  • the dialysis ion solution will be transferred to the next sericin hydrolysis; the hydrolysis end point is passed.
  • the UV-Vis spectrophotometer compares the transmittance of the test hydrolysate to determine;
  • step 2) Dissolve the silk fibroin fibers filtered in step 2) in a neutral salt solution with a temperature of 60-100 ° C and a mass percentage of 30-60% to form a silk fibroin protein solution;
  • Step 4) hydrolyzed silk fibroin protein solution was electrodialyzed to remove ions from the solution, and the conductivity of the solution was reduced to 10-500us / cm to obtain a pale yellow silk protein pure solution.
  • the ionic solution can be recycled as a neutral solution in step 4);
  • step 6) Mix the sericin hydrolysate of step 3) and the pure solution of silk protein of step 5) uniformly, that is, prepare a novel silk protein hydrolysate with surfactant characteristics.
  • the degumming agent uses sodium carbonate or sodium bicarbonate aqueous solution; the hydrolysis temperature is 50-80 ° C, and the time is 2-4 hours;
  • control of the hydrolysis end point of the silk protein described in step 3) is to determine the end point of hydrolysis by testing the transmittance of the hydrolysate with an ultraviolet-visible spectrophotometer to obtain a molecular weight of 10,000-200,000 Daltons , Silk hydrolysed protein with the best molecular weight in the range of 100,000-200,000 Daltons, so that the final product has the best foaming, foam stabilizing, moisturizing, scalp repairing effects.
  • the neutral salt solution is a CaCl 2, CaCl 2 -H 2 O, CaCl 2 -2H 2 O, or LiBr solution.
  • the invention also provides a preparation method of the anti-dandruff anti-itch shampoo and hair care composition containing the silk protein component, comprising the following steps:
  • a scalp anti-dandruff anti-itching method when shampooing, the anti-dandruff anti-itch shampoo and hair care composition used the anti-dandruff anti-itch shampoo and hair care composition containing the silk protein component
  • the antidandruff antipruritic shampoo and hair care composition prepared by the preparation method has a scalp micro-ecological environment composed of physiological lipids, natural moisturizing factors and scalp microbial populations.
  • the present invention has the following advantages and beneficial technical effects:
  • the silk protein hydrolysate obtained by the silk protein hydrolysis process used in the present invention is based on the theory of how to maintain the micro-ecological environment of the scalp, and uses the special moisturizing and repairing functions of the silk hydrolysate to solve the problem of dryness and deficiency of the scalp Start with problems such as water and brittle hair, and solve the physiological causes of dandruff from the source.
  • the simultaneous application of the two mechanisms has a synergistic effect on better inhibiting the production of dandruff; by improving the skin's moisturizing performance, the scalp's microscopic scalp composed of physiological lipids, natural moisturizing factors, and scalp microbial population is improved Ecological environment, maintain scalp health, and achieve anti-dandruff and itching effect.
  • the anti-dandruff anti-itch shampoo and hair care composition using the silk protein component obtained by the present invention can obtain an anti-dandruff effect without adding any Chinese herbal medicines or synthetic fungicides; It can be seen from the test results that the shampoo prepared by the formula without any anti-dandruff and anti-itch ingredients also has anti-dandruff and anti-itch effects.
  • the clean scalp can also be maintained for 3-4 days.
  • the formula is combined with an appropriate Chinese herbal medicine fungicide or synthetic fungicide to solve the problem of dandruff caused by excessive reproduction of microorganisms. Both mechanisms The application has a synergistic effect on better inhibiting the production of dandruff, and has the characteristics of simple formula and excellent use effect.
  • FIG. 1 is a schematic diagram of the distribution range of the main molecular weight of the silk hydrolysate of the present invention from 20,000 to 200,000 Daltons.
  • FIG. 2 is a graph showing the test results of the compatibility of silk hydrolysate and other surfactants according to the present invention.
  • Fig. 3 is a graph of the scalp effect of the anti-dandruff anti-itch shampoo and hair care composition of the present invention before and after use.
  • Moisturizing factors such as filaggrin and its degradation products maintain the moisture content of the stratum corneum, maintain the pH weak acid environment of the stratum corneum, strengthen the adhesion of the intercellular substance, and thus maintain the balance of the flora on the skin surface ;
  • the normal reproduction of the scalp microbial population and the decomposition of dandruff can be converted into some moisturizing factors.
  • a large number of hydrophilic groups appear on the side chain of the hydrolyzed silk protein after its decomposition, thereby obtaining good hygroscopicity and enhancing the moisture retention of the scalp.
  • the sericin and small molecular keratin obtained by the silk protein hydrolysis process described in the present invention can form a "mud" cell adhesion substance on the surface of the scalp, which can repair the epidermal cells that are about to be peeled off and delay the exfoliation of the scalp. At the same time, it can repair the hair shaft and prevent or reduce hair breakage.
  • the silk protein hydrolysate obtained by the silk protein hydrolysis process of the present invention has a certain inhibitory effect on Malassezia furfur.
  • the irritation of the conventional surfactants used in the shampoo is one of the factors for the formation of dandruff.
  • the stimulation of the scalp by some foaming agents in the shampoo accelerates and increases the production of dandruff.
  • the silk protein hydrolysate obtained by the silk protein hydrolysis process described in the present invention can effectively prevent or reduce the irritation of the foaming agent to the scalp, thereby further reducing dandruff.
  • the main principles of the present invention are: improving skin moisturizing performance, improving the scalp micro-ecological environment composed of physiological lipids, natural moisturizing factors, scalp microbial population, maintaining scalp health, and using silk protein hydrolysis process
  • the obtained silk protein hydrolysate has a certain inhibitory effect on Malassezia furfur, and it can effectively prevent or reduce the irritation of the foaming agent on the scalp, and achieve the effect of anti-dandruff and itching.
  • the invention provides an anti-dandruff anti-itch shampoo and hair care composition containing silk protein components, which comprises the following components in weight ratio:
  • the silk protein hydrolysate added to the anti-dandruff antipruritic shampoo and hair care composition containing the silk protein component of the present invention enhances the moisture retention of the scalp, repairs and improves the adhesion between keratinocytes of the scalp, and improves the physiological lipid of the scalp , Natural moisturizing factor, scalp micro-ecological environment composed of microbial population of scalp, so as to achieve the technical effect of slowing down or reducing the formation of dandruff.
  • the retention moisturizing ingredient of the skin which is not easy to rinse is added to the formulation, in particular, the silk protein hydrolysate obtained through a special process is preferably added.
  • silk is mainly composed of two components: sericin and silk fibroin.
  • sericin is mainly collagen
  • silk fibroin is keratin.
  • Silk contains 18 kinds of amino acids, including 10 kinds of essential or semi-essential amino acids. Because sericin and silk fibroin need to be hydrolyzed under different hydrolysis conditions, we used a two-step hydrolysis method to obtain a silk protein hydrolysate containing both sericin and keratin.
  • the silk used exclusively for cosmetics needs to meet the following conditions:
  • the silkworm is a second-generation silkworm obtained from the sericulture technology station.
  • the silkworm is used to stabilize the content of the sericin and silk fibroin, so as to obtain a stable hydrolysis ratio of hydrolyzed sericin and hydrolyzed silk fibroin. product.
  • the culture environment of silkworm is related to microbial control of later products and silkworm leaf disease.
  • the silkworm breeding environment is aseptic, ventilated, and dry silkworm breeding in order to reduce the risk of germs and microorganisms in the final product.
  • Silk is an active protein and needs to be stored in a cool, dry and ventilated place.
  • a good quality silk raw material is required to do quality control in all aspects. From the selection of silkworms to breeding; from the cultivation of mulberry leaves to the feeding of silkworms; from mature silkworms to cocooning; from storage to transportation; especially the hydrolysis process control of silk, can be controlled by different processes, not only can be very good Can retain the activity of silk protein, and can obtain hydrolyzed silk protein with different molecular weight and different functions.
  • a preparation process of silk protein hydrolysate includes the following steps:
  • the whole silk hydrolysate of this embodiment is a novel silk protein hydrolysate with surfactant characteristics.
  • the light yellow all-silk hydrolysate of this embodiment has a main molecular weight ranging from 20,000 to 200,000 Daltons.
  • the product has a lubricating feel, good water retention, and has a certain degree of foaming. It has a good foaming and stabilizing effect when combined with other surfactants.
  • a preparation process of silk protein hydrolysate includes the following steps:
  • the whole silk hydrolysate of this embodiment is a novel silk protein hydrolysate with surfactant characteristics.
  • the light yellow all-silk hydrolysate of this embodiment has a main molecular weight range of 50,000-200,000 Daltons; the product has a smooth hand feel, good water retention, and a certain degree of foaming. It has a good combination with other surfactants. Foam increasing and stabilizing effect.
  • a preparation process of silk protein hydrolysate includes the following steps:
  • the whole silk hydrolysate of this embodiment is a novel silk protein hydrolysate with surfactant characteristics.
  • the light yellow all-silk hydrolysate of this embodiment has a main molecular weight ranging from 100,000 to 200,000 Daltons; the product has a smooth feel, good water retention, and has certain foaming properties and other surfactants (such as coconut oil-based grapes) Glycoside, sodium lauryl glycoside sodium carboxylate, lauryl glycoside, fatty alcohol polyoxyethylene ether) compound has a good foam stabilizing effect.
  • surfactants such as coconut oil-based grapes
  • Test results During the observation period, there was no skin irritation reaction of erythema and edema in the skin of the New Zealand rabbits tested, and the score value of each animal in the sample group was 0 points per day The results of the sex test are shown in Table 1 below).
  • the solution compounded with the silk hydrolysate according to the present invention increased the amount of foam obtained after shaking with equal force and equal duration, and the density of the foam was significantly strengthened. And the residual amount of foam after standing for 6 hours is equal to or more than the residual amount of foam after using surfactant alone for 4 hours.
  • the silk hydrolysate involved in the present invention has good foaming and stability when compounded with other surfactants Bubble effect.
  • the silk protein hydrolysate obtained by the silk protein hydrolysis process of the present invention has a certain inhibitory effect on Malassezia furfur.
  • the silk protein hydrolysate obtained by the protein hydrolysis process has an inhibition rate of 14% and 24% respectively against Malassezia furfur.
  • the shampoo prepared by the formula without any anti-dandruff and anti-itch ingredients also has anti-dandruff and anti-itch effects, and the clean scalp can also maintain 3-4 day. From this, it can be concluded that the generation of dandruff is directly related to scalp drying and scalp maintenance.
  • the technical solution of the anti-dandruff anti-itch shampoo and nourishing composition of the present invention has the advantage that, by adding only a silk hydrolysate verification formula, it is verified that the anti-dandruff anti-itch fungicide can also achieve the anti-dandruff anti-itch effect The fact that this is unprecedented in existing products of this type.
  • the deionized water in the raw material components is the solvent; disodium ethylenediaminetetraacetic acid is the metal chelating agent stabilizing system; the citric acid PH adjusting agent; glycerin common moisturizer; AESA surfactant is the main blowing agent; Imidazoline is a foam booster; sodium olefin sulfonate is a foam booster and foam stabilizer; diethanolamide is a foam booster and foam stabilizer; cellulose acetate butyrate is a thickening stabilizer; silk hydrolysate is a moisturizing conditioner and can enhance the scalp Moisturizing and improve the micro-ecological environment of the scalp, so as to achieve the purpose of inhibiting the formation of dandruff; carcassone is a preservative; flavor is a flavoring agent; sodium chloride is a thickening stabilizer.
  • the silk hydrolysate obtained by the production process of the present invention is added to the formula.
  • the main feature of the silk hydrolysate is that the molecules of the silk hydrolysate protein are concentrated in the range of 20,000-200,000 Daltons. , A small and medium molecule protein.
  • An anti-dandruff anti-itch shampoo and hair care composition containing silk protein components comprising the following components in weight ratio:
  • the raw materials of the above components are mixed at room temperature, water and disodium edetate are added to the pot and stirred to dissolve; AESA, imidazoline, sodium olefin sulfonate, diethanolamide, glycerin, Cellulose acetate butyrate dissolves completely and transparently; then add carcassone and flavor to dissolve completely and transparently; finally add silk hydrolysate silk, stir well, add salt to adjust viscosity (25 °C): 5000, add citric acid to adjust PH value 5.8- 6.5 is enough.
  • AESA imidazoline, sodium olefin sulfonate, diethanolamide, glycerin, Cellulose acetate butyrate dissolves completely and transparently; then add carcassone and flavor to dissolve completely and transparently; finally add silk hydrolysate silk, stir well, add salt to adjust viscosity (25 °C): 5000, add citric acid to adjust PH value 5.8- 6.5 is enough.
  • An anti-dandruff anti-itch shampoo and hair care composition containing silk protein components comprising the following components in weight ratio:
  • Deionized water 85g, ethylenediaminetetraacetic acid disodium (EDTA-2Na) 0.1g, citric acid 0.2g, glycerin 3g, AESA surfactant 15g, imidazoline 3g, sodium olefin sulfonate (AOS) 3 grams, 3 grams of diethanolamide (6501), 3 grams of cellulose acetate butyrate (CAB), 7 grams of silk hydrolysate of Example 2, 0.1 grams of carcassone, 0.1 grams of flavor, and an appropriate amount of sodium chloride.
  • EDTA-2Na ethylenediaminetetraacetic acid disodium
  • citric acid 0.2g glycerin 3g
  • AESA surfactant 15g imidazoline 3g, sodium olefin sulfonate (AOS) 3 grams, 3 grams of diethanolamide (6501), 3 grams of cellulose acetate butyrate (CAB), 7 grams of silk hydrolysate of Example 2, 0.1 grams of carcas
  • the raw materials of the above components are mixed at room temperature, water and disodium edetate are added to the pot and stirred to dissolve; AESA, imidazoline, sodium olefin sulfonate, diethanolamide, glycerin, Cellulose acetate butyrate dissolves completely and transparently; then add carcassone and flavor to dissolve completely and transparently; finally add silk hydrolysate silk, stir well, add salt to adjust viscosity (25 °C): 5000, add citric acid to adjust PH value 5.8- 6.5 is enough.
  • AESA imidazoline, sodium olefin sulfonate, diethanolamide, glycerin, Cellulose acetate butyrate dissolves completely and transparently; then add carcassone and flavor to dissolve completely and transparently; finally add silk hydrolysate silk, stir well, add salt to adjust viscosity (25 °C): 5000, add citric acid to adjust PH value 5.8- 6.5 is enough.
  • An anti-dandruff anti-itch shampoo and hair care composition containing silk protein components comprising the following components in weight ratio:
  • the raw materials of the above components are mixed at room temperature, water and disodium edetate are added to the pot and stirred to dissolve; AESA, imidazoline, sodium olefin sulfonate, diethanolamide, glycerin, Cellulose acetate butyrate dissolves completely and transparently; then add carcassone and flavor to dissolve completely and transparently; finally add silk hydrolysate silk, stir well, add salt to adjust viscosity (25 °C): 5000, add citric acid to adjust PH value 5.8- 6.5 is enough.
  • AESA imidazoline, sodium olefin sulfonate, diethanolamide, glycerin, Cellulose acetate butyrate dissolves completely and transparently; then add carcassone and flavor to dissolve completely and transparently; finally add silk hydrolysate silk, stir well, add salt to adjust viscosity (25 °C): 5000, add citric acid to adjust PH value 5.8- 6.5 is enough.
  • the invention adds silk hydrolysate to the formulation, which is a retention type and is not easy to rinse the skin moisturizing ingredients. It uses the main two components of silk, sericin and silk fibroin. Sericin is mainly collagen and silk fibroin. Protein, 18 kinds of amino acids contained in silk, among which 10 kinds of essential or semi-essential amino acids are contained in sericin and silk fibroin. The verification formula of only adding silk hydrolysate has verified that no dandruff is added. The fact that itching fungicides can also achieve anti-dandruff and itching effects.
  • the formula of the embodiment of the present invention can be mixed by adding any shampoo on the market; it can also be added to the formula of the present invention with appropriate Chinese herbal medicine fungicides or synthetic fungicides to solve the problem caused by excessive proliferation of microorganisms
  • the dandruff problem, the two mechanisms are applied at the same time, and it has a synergistic effect on better inhibiting the production of dandruff.
  • anti-dandruff anti-itch shampoo and hair care compositions of Examples 4-6 of the present invention were subjected to microbial, hygienic and chemical testing items according to the 2015 edition of the "Cosmetic Safety Technical Specifications”.
  • test results show that three samples (products of Examples 4-6) were inspected for hygiene and safety according to the 2015 edition of the "Cosmetics Safety Technical Specifications", as follows:
  • Microbiological examination the test results of total colonies, total molds and yeasts, heat-resistant coliforms, Staphylococcus aureus, Pseudomonas aeruginosa all meet the requirements;
  • Test items test result Limit Total number of colonies (CFT / g) ⁇ 10 ⁇ 1000 Total mold and yeast (CFT / g) ⁇ 10 ⁇ 100 Heat-resistant coliform / g not detected Not detectable Staphylococcus aureus / g not detected Not detectable Pseudomonas aeruginosa / g not detected Not detectable
  • test effect of the anti-dandruff effect of the silk anti-dandruff shampoo and hair care composition is shown in Table 5 below.
  • hair types are divided into oily, dry, neutral and damaged hair; the following are introduced separately.
  • Oily greasy hair, sticky touch, dandruff, lack of luster
  • Damaged hair Dry hair, rough touch, lack of luster, and yellowish color.
  • the template prepared by the verification formula of the present invention is randomly selected and used by 12 volunteers, which can improve dandruff and scalp itching to a certain extent.
  • the present invention improves the scalp micro-ecological environment composed of physiological lipids, natural moisturizing factors, and scalp microbial populations by improving skin moisturizing performance, maintaining scalp health, and achieving dandruff Itching effect.

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Abstract

一种含蚕丝蛋白成分的去屑止痒洗发养发组合物及其制备方法，该去屑止痒洗发养发组合物包括以下重量比的组分：去离子水70-85份、乙二胺四乙酸二钠0.1-03份、柠檬酸0.2-0.4份、甘油1-3份、AESA表面活性剂10-15份、咪唑啉1-3份、烯烃磺酸钠1-3份、二乙醇酰胺1-3份、醋酸丁酸纤维素2-4份、蚕丝蛋白水解液1-8份、卡松0.1-0.3份、香精0.1-0.3份、氯化钠适量。

Description

一种含蚕丝蛋白成分的去屑止痒洗发养发组合物及其制备方法 技术领域
本发明涉及一种洗发养发组合物，属于化学护理用品技术领域，具体涉及一种含蚕丝蛋白成分的去屑止痒洗发养发组合物及其制备方法。
背景技术
头皮屑是人类常见的一种生理现象，是一种反复性多发性皮肤问题。头屑增多不但会伴随着头皮瘙痒，给人带来不适，特别是，满头的头屑也非常影响美观。传统去屑止痒理论多认为：头皮屑的产生是因为糠秕马拉色菌等真菌类引起的。大家的研究重点就是如何用更好的杀菌剂来抑制或杀灭这些微生物。
因此，各形各色种类繁多的具有杀菌作用的去屑止痒成分被应用到去屑止痒洗发水产品中。在这些洗发水配方中加入诸如：甘宝素、ZPT、OTC等合成杀菌剂，或是金银花、香茅、茶树油、苦参等植物类杀菌剂，但即使这样，还是没有一款产品能较好地解决头屑与头皮瘙痒的问题。因为，忽视了头皮形成的另一个关键因素-皮肤干燥所引起的头屑与头皮瘙痒。
事实上，经研究发现人体头皮表面有一个由生理脂质、天然保湿因子、微生物种群等构成的一个生态平衡的微生态环境，维护头皮的微生态环境平衡、健康就可以保证头皮也就健康。
因此，要维护我们的头皮微生态平衡，在我们设计去头屑的产品配方的时候，就该从维持生理油脂平衡、头皮保湿、维持头皮微生物种群的稳定性等方面着手。现有技术的洗发水产品没有考虑到从维护头皮微生态平衡着手、去设计去头屑的产品配方，没有从如何解决头皮发干、缺水等技术问题着手，从源头上解决头皮屑产生的生理因素。
众所周知，蚕丝是由外面的一层丝胶以及里层的一层丝素构成。不论是丝胶为蚕丝胶蛋白，丝素是角蛋白，都是上好的天然护肤材料。但是，鉴于现今的蚕丝主要应用于纺织品工业，没有专门为化妆品开发和养殖的桑蚕，因此，就带来了许多诸如产品原料杂质太多、过敏率高等问题。
但是，以蚕丝蛋白水解原料作为去头皮屑的主要成分的报道还没有出现过。
发明内容
由于现有技术存在的问题，本发明的目的是提供一种含蚕丝蛋白成分的去屑止痒洗发 养发组合物，通过使用带有含蚕丝蛋白成分的洗发液，改善和维护头皮微生态环境的理论为基础，综合考虑增强头皮的保湿性、与适当抑制头皮微生物种群的正常水平两种因素，解决微生物过量繁殖引起的头屑问题。
本发明的另一目的是提供一种含上述蚕丝蛋白成分的去屑止痒洗发养发组合物的制备方法。
本发明所采用的技术方案如下：
一种蚕丝蛋白水解液的制备方法，包括以下步骤：
1)选择个大壳厚的优质种蚕的蚕茧并去除蚕茧中的蚕蛹、蚕衣与杂质，绞碎备用；
2)使用0.1-1％的碳酸钠或碳酸氢钠溶液作为脱胶剂，其茧量为0.4-10％，水解温度控制在50-100℃水浴温度下脱胶2-4h，过滤得到水解蚕丝胶蛋白(滤液)和丝素蛋白纤维(滤渣)；所得滤液通过电渗析装置脱盐，得到的脱盐水解蚕丝胶蛋白留用，所脱出的盐溶液，可以用于下一次水解，从而减少排放，降低成本，减少污染；
3)将丝素蛋白纤维滤渣溶解在质量比浓度为30-50％的中性盐溶液中，温度为80-100℃；水解终点通过紫外可见分光光度计比较测试水解液的透光率来判定；
4)将水解好的丝素蛋白液进行电透析，除掉溶液中的杂离子，循环至溶液的电导率为100-500us/cm，得到浅黄色丝蛋白纯溶液；分离出的电解质溶液可以用于下一次水解生产用；
5)最后将质量浓度为1-5％的丝素蛋白液和1-5％的丝胶蛋白液混合，获得蛋白质分子量为2万-20万道尔顿的全蚕丝水解液。
进一步而言，步骤1)中，所述蚕茧的培育方法为：
1)桑田的选择：
选择阳光充足、昼夜温差大的云南山区种植桑树，桑叶含糖量高，有利于蚕宝宝的健康成长，从而获得壳厚个大的优质茧壳，另外，云南山区独特的小盆地结构，形成了一个天然的屏障，从而减少非养蚕区的农药飘散到养蚕区，从而对终产物的农药残留有保障；
2)种蚕的精选：
种蚕是从蚕业技术站获得的二代蚕，采用种蚕是为了所获得的蚕丝胶蛋白与丝素蛋白的含量稳定，从而获得水解蚕丝胶蛋白与水解丝素蛋白比较稳定比例的水解终产品；
3)养殖环境：
桑蚕的养殖环境于后期产品的微生物控制以及蚕叶病相关；在本发明中，所述桑蚕的养殖环境是采用无菌、通风、干燥的蚕室内养殖，以降低最终产品的病菌、微生物等风险；
4)储存条件：
蚕丝是活性蛋白，需要在阴凉、干燥、通风处储存。
进一步而言，步骤3)中，所述中性盐溶液选自质量比浓度为30-50％的无水CaCl 2、CaCl 2-H 2O、CaCl 2-2H 2O或LiBr溶液。
进一步而言，步骤3)中，所述对水解终点的控制，是保证步骤5)所获得的终产物的蚕丝蛋白的分子量控制在2万-20万道尔顿的区间范围，主要集中在10万-20万道尔顿区间范围，而非其他专利或者工艺所获得的水解产物为蚕丝肽或氨基酸；终产物分子量的控制是本发明产品所获得的产品功效性的保证。
另外，一种含蚕丝蛋白成分的去屑止痒洗发养发组合物，包括以下重量比的组分：
去离子水70-85份、乙二胺四乙酸二钠0.1-0.3份、柠檬酸0.2-0.4份、甘油1-3份、AESA表面活性剂10-15份、咪唑啉1-3份、烯烃磺酸钠1-3份、二乙醇酰胺1-3份、醋酸丁酸纤维素2-4份、蚕丝蛋白水解液1-8份、卡松0.1-0.3份、香精0.1-0.3份、氯化钠适量。
上述含蚕丝蛋白成分的去屑止痒洗发养发组合物，所述蚕丝蛋白水解液是通过以下工艺制备得到：
1)按照常规方法，使用弱碱性水溶液作为脱胶剂对蚕茧脱胶，在脱胶剂溶液质量百分数为0.4-6％，pH为8-11，水解温度为50-100℃的条件下对蚕茧脱胶；
2)过滤步骤1)的溶液，形成脱胶水解液和蚕丝丝素纤维；
3)将步骤2)滤出的脱胶水解液通过电渗析后分成丝胶水解液和渗析离子溶液，将丝胶水解液留住，渗析离子溶液将转入下一次丝胶水解用；水解终点通过紫外可见分光光度计比较测试水解液的透光率来判定；
4)将步骤2)滤得的蚕丝丝素纤维溶解在温度为60-100℃，质量百分数为30-60％的中性盐溶液中，形成蚕丝丝素蛋白液；
5)将步骤4)水解好的蚕丝丝素蛋白液进行电透析除掉溶液中的离子，循环至溶液的电导率降至10-500us/cm，得到浅黄色蚕丝蛋白纯溶液，电透析后的离子溶液可循环作为步骤4)中的中性溶液使用；
6)将步骤3)的丝胶水解液和步骤5)的蚕丝蛋白纯溶液混合均匀，即制得具有表面活性剂特性的新型蚕丝蛋白质水解液。
进一步而言，步骤1)中，所述脱胶剂采用碳酸钠或碳酸氢钠水溶液；所述水解温度为50-80℃，时间为2-4小时；
进一步而言，步骤3)中所述的蚕丝蛋白的水解终点控制，在于通过紫外可见分光光度计测试水解液的透光率而判定水解的终点，从而获得分子量在1万-20万道尔顿，最佳分子量在10万-20万道尔顿范围的蚕丝水解蛋白，从而使终产品具有最佳的起泡性、稳泡性、保湿性、头皮修护作用等功效。
进一步而言，步骤4)所述中性盐溶液为CaCl 2、CaCl 2-H 2O、CaCl 2-2H 2O或者LiBr溶液。
另外，本发明还提供一种上述含蚕丝蛋白成分的去屑止痒洗发养发组合物的制备方法，包括以下步骤：
1)将上述组分的原料在室温下混合，先将水、乙二胺四乙酸二钠加入锅中搅拌，溶解；
2)依次加入AESA、咪唑啉、烯烃磺酸钠、二乙醇酰胺、甘油、醋酸丁酸纤维素溶解完全透明；
3)依次加入卡松、香精溶解完全透明；
4)最后，加入蚕丝蛋白水解液丝，搅拌均匀，加入盐调节好粘度(25℃)：5000，加入柠檬酸调节PH值5.8-6.5即可。
进一步而言，一种头皮去屑止痒的方法，在洗发时，所使用的去屑止痒洗发养发组合物采用上述含蚕丝蛋白成分的去屑止痒洗发养发组合物的制备方法所制备得到的去屑止痒洗发养发组合物，其具有改善头皮的生理脂质、天然保湿因子、头皮微生物种群所组成的头皮微生态环境。
借由上述技术方案，本发明具有如下优点和有益技术效果：
1)本发明采用的蚕丝蛋白水解工艺所获得的蚕丝蛋白水解液以如何维护头皮微生态环境的理论为基础，利用蚕丝水解物的特殊的保湿与修护理功能，从如何解决头皮发干、缺水、头发易断等问题着手，从源头上解决头皮屑产生的生理原因。
2)另外，我们通过采用不同浓度的蚕丝水解液测试其对大家所公认的影响头皮屑的主要微生物糠秕马拉色菌的抑制作用，发现3％、4％这两种不同浓度的采用本发明所描述的蚕丝蛋白水解工艺所获得蚕丝蛋白水解液，分别对糠秕马拉色菌具有14％与24％的抑制率。
从而，两种机理同时应用，对更好地抑制头皮屑的产生起到协同增效的效果；通过提高皮肤保湿性能，改善头皮由生理脂质、天然保湿因子、头皮微生物种群所组成的头皮微生态环境，维护头皮健康，而达到去屑止痒的效果。
3)采用本发明所得到的含蚕丝蛋白成分的去屑止痒洗发养发组合物在不添加任何中草药类的或合成的杀菌剂的情况下，能获得去头皮屑的效果；从多次试验的结果可以看出，用不加任何去屑止痒成分的配方所调制出的洗发水，同样具有去屑止痒效果。
而且，干净的头皮还可以维持3-4天，在实际的生产配方中，在配方中配合适当的中草药类的杀菌剂或合成杀菌剂，解决微生物过量繁殖引起的头屑问题，两种机理同时应用，对更好地抑制头皮屑的产生起到协同增效的效果，具有配方简单，使用效果优良的特点。
附图说明
图1是本发明蚕丝水解液的主要分子量2万-20万道尔顿的分布范围示意图。
图2是本发明所涉及的蚕丝水解液与其他表面活性剂复配性测试效果图。
图3是本发明去屑止痒洗发养发组合物分别在使用前和使用后的头皮效果图。
具体实施方式
下面对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
我们发现，头皮表面的生态环境是由生理脂质、头皮屑、保湿因子，微生物种群等共同构建的。微生物不一定是头皮角质脱落加速的主要因素。生理脂质、丝聚蛋白等保湿成分的缺失对头皮屑的产生以及加速脱落是重要原因。我们可以通过构建或保护头皮表面的健康的生态环境来达到去屑止痒的目的：
1)生理脂质与丝聚蛋白协同构建头皮表皮的屏障；
2)丝聚蛋白和它的降解产物等保湿因子，保持了角质层的含水量，维持了角质表层的pH弱酸环境，加强了细胞间质的黏连作用，进而维持了皮肤表面的菌群平衡；头皮微生物种群的正常繁殖以及对头屑的分解可以转化为部分保湿因子。
3)水解的蚕丝蛋白因其分解后的侧链上出现了大量的亲水基团，从而获得了很好的吸湿性，可以增强头皮的保湿性。采用本发明所述的蚕丝蛋白水解工艺所获得的蚕丝胶蛋白与小分子角蛋白可以在头皮表面形成“泥浆”类细胞黏连物质，可以修复即将剥离的表皮细胞，延缓头皮的脱落。同时可以修复发干，防止或减少头发断裂。
4)采用本发明的蚕丝蛋白水解工艺所获得的蚕丝蛋白水解液对糠秕马拉色菌具有一定的抑制作用。
5)洗发水中所采用的常规表面活性剂的刺激性是头皮屑形成的因素之一，洗发水中的部分发泡剂对头皮的刺激，加快并增多了头皮屑的产生。采用本发明所描述的蚕丝蛋白水解工艺所获得的蚕丝胶蛋白水解液可以有效阻止或降低发泡剂对头皮的刺激性，从而也进一步地减少了头皮屑。
综上所述，本发明主要原理是：提高皮肤保湿性能，改善头皮由生理脂质、天然保湿因子、头皮微生物种群所组成的头皮微生态环境，维护头皮健康，以及采用的蚕丝蛋白水解工艺所获得的蚕丝蛋白水解液对糠秕马拉色菌具有一定的抑制作用，及其可以有效阻止或降低发泡剂对头皮的刺激性，而达到去屑止痒的效果。
本发明提供了一种含蚕丝蛋白成分的去屑止痒洗发养发组合物，包括以下重量比的组分：
去离子水70-85份、乙二胺四乙酸二钠0.1-0.3份、柠檬酸0.2-0.4份、甘油1-3份、AESA 表面活性剂10-15份、咪唑啉1-3份、烯烃磺酸钠1-3份、二乙醇酰胺1-3份、醋酸丁酸纤维素2-4份、蚕丝蛋白水解液1-8份、卡松0.1-0.3份、香精0.1-0.3份、氯化钠适量。
本发明所述含蚕丝蛋白成分的去屑止痒洗发养发组合物加入的蚕丝蛋白水解液，增强头皮的保湿性，修复并改善头皮角质细胞之间的黏连，改善头皮的生理脂质、天然保湿因子、头皮微生物种群所组成的头皮微生态环境，从而达到减缓或减少头皮屑生成的技术功效。
本发明的技术关键以及与其他专利申请的不同点，就是在配方中加入了滞留型，不易轻易冲洗的皮肤保湿成分，特别是，优选加入了经过特殊工艺获得的蚕丝蛋白水解液。众所周知，蚕丝主要由两种成分组成：丝胶与丝素。其中，丝胶主要为胶原蛋白，丝素为角蛋白。蚕丝中含有18种氨基酸，其中人体所必需的或半必需的氨基酸10种。因为丝胶与丝素需要在不同的水解条件下水解，因此我们采用两步水解法，获得了既含蚕丝胶蛋白又含角蛋白的蚕丝蛋白水解液。
以下将分别介绍蚕丝的原料来源以及蚕丝蛋白水解液的制备工艺。
一、蚕丝的原料来源
本发明选择用化妆品专用蚕丝，其需要满足以下条件：
1、桑田的选择
选择阳光充足、昼夜温差大的云南山区种植桑树，桑叶含糖量高，有利于蚕宝宝的健康成长，从而获得壳厚个大的优质茧壳，另外，云南山区独特的小盆地结构，形成了一个天然的屏障，从而减少非养蚕区的农药飘散到养蚕区，从而对终产物的农药残留有保障；
2、种蚕的精选
种蚕是从蚕业技术站获得的二代蚕，采用种蚕是为了所获得的蚕丝胶蛋白与丝素蛋白的含量稳定，从而获得水解蚕丝胶蛋白与水解丝素蛋白比较稳定比例的水解终产品。
3、养殖环境
桑蚕的养殖环境于后期产品的微生物控制以及蚕叶病相关。在本发明中，所述桑蚕的养殖环境是采用无菌、通风、干燥的蚕室内养殖，以降低最终产品的病菌、微生物等风险。
4、储存条件
蚕丝是活性蛋白，需要在阴凉、干燥、通风处储存。
二、蚕丝蛋白水解液的生产工艺与品质控制：
一种好品质的蚕丝原料是需要做好各个环节的品质控制。从种蚕的挑选到育种；从桑叶的种植到桑蚕的喂养；从熟蚕到结茧；从储存到运输；特别是蚕丝的水解工艺控制，可 以通过不同的工艺控制，不但可以很好的保留蚕丝蛋白活性，而且可以获得不同分子量不同功能的水解蚕丝蛋白。
实施例1(蚕丝蛋白水解液的制备工艺)
一种蚕丝蛋白水解液的制备工艺，包括以下步骤：
1)选择个大壳厚的优质种蚕蚕茧10g并去除蚕茧中的蚕蛹，将蚕茧摘除蚕衣洗净杂质，绞碎备用；
2)使用90克1％的碳酸钠溶液作为脱胶剂，水解温度控制在50-80℃水浴温度下脱胶4h，过滤得到水解滤液和丝素蛋白纤维(滤渣)；
3)将丝素蛋白纤维滤渣溶解在质量比浓度为30％的无水CaCl 2溶液中，温度为60-100℃；当透光率达到40％左右的时候，停止水解；
4)将水解好的丝素蛋白液在半渗透膜渗透袋中进行电透析，除掉溶液中的杂离子，循环至溶液的电导率为100us/cm，得到浅黄色丝蛋白纯溶液；
5)将脱胶得到的脱胶水溶液同时进行电渗析至电导率降低至丝胶溶液100us/cm，得到浅黄色丝胶溶液；
6)最后将丝素蛋白液和丝胶蛋白液混合，得到分子量范围为2万-20万道尔顿，手感润滑，保水性好的全蚕丝水解液。
本实施例的全蚕丝水解液也就是制得了具有表面活性剂特性的新型蚕丝蛋白质水解液。
如图1所示，本实施例的浅黄色全蚕丝水解液其主要分子量范围为2万-20万道尔顿。产品手感润滑，保水性好，且具有一定的发泡性与其他表面活性剂复配具有很好的增泡稳泡作用。
实施例2(蚕丝蛋白水解液的制备工艺)
一种蚕丝蛋白水解液的制备工艺，包括以下步骤：
1)选择个大壳厚的优质种蚕蚕茧20g并去除蚕茧中的蚕蛹，将蚕茧摘除洗净杂质，绞碎备用；
2)使用150克的0.5％的碳酸氢钠溶液作为脱胶剂，水解温度控制在50-80℃水浴温度下脱胶3h，过滤得到水解滤液和丝素蛋白纤维(滤渣)；
3)将丝素蛋白纤维滤渣溶解在质量比浓度为50％的无水CaCl 2溶液中，温度为60-100℃；当透光率达到35％左右的时候，停止水解；
4)将水解好的丝素蛋白液在半渗透膜渗透袋中进行电透析，除掉溶液中的杂离子，循 环至溶液的电导率为500us/cm，得到浅黄色丝蛋白纯溶液；
5)将脱胶得到的脱胶水溶液同时进行电渗析至电导率降低至丝胶溶液500us/cm，得到浅黄色丝胶溶液；
6)最后将丝素蛋白液和丝胶蛋白液混合，得到分子量为5万-20万道道尔顿；手感润滑保水性好的全蚕丝水解液。
本实施例的全蚕丝水解液也就是制得了具有表面活性剂特性的新型蚕丝蛋白质水解液。
本实施例的浅黄色全蚕丝水解液其主要分子量范围为5万-20万道道尔顿；产品手感润滑，保水性好，且具有一定的发泡性与其他表面活性剂复配具有很好的增泡稳泡作用。
实施例3(蚕丝蛋白水解液的制备工艺)
一种蚕丝蛋白水解液的制备工艺，包括以下步骤：
1)选择个大壳厚的优质种蚕蚕茧30g并去除蚕茧中的蚕蛹，将蚕茧摘除洗净杂质，绞碎备用；
2)使用200克的5％的碳酸氢钠溶液作为脱胶剂，水解温度控制在50℃水浴温度下脱胶4h，过滤得到水解滤液和丝素蛋白纤维(滤渣)；
3)将丝素蛋白纤维滤渣溶解在质量比浓度为60％的无水CaCl 2溶液中，温度为100℃；当透光率达到50％左右的时候，停止水解；
4)将水解好的丝素蛋白液在半渗透膜渗透袋中进行电透析，除掉溶液中的杂离子，循环至溶液的电导率为400us/cm，得到浅黄色丝蛋白纯溶液；
5)将脱胶得到的脱胶水溶液同时进行电渗析至电导率降低至丝胶溶液400us/cm，得到浅黄色丝胶溶液；
6)最后将丝素蛋白液和丝胶蛋白液混合，得到分子量为10万-20万道道尔顿；功能怎样的全蚕丝水解液。
本实施例的全蚕丝水解液也就是制得了具有表面活性剂特性的新型蚕丝蛋白质水解液。
本实施例的浅黄色全蚕丝水解液其主要分子量范围为10万-20万道道尔顿；产品手感润滑，保水性好，且具有一定的发泡性与其他表面活性剂(如椰油基葡萄苷、月桂基糖苷羧酸钠和月桂基糖苷、脂肪醇聚氧乙烯醚)复配具有很好的增泡稳泡作用。
效果试验例1(皮肤刺激性)
1、多次皮肤刺激性试验(由广东省保化检测中心提供的检测报告)。
2、检测依据：《化妆品安全技术规范》2015年版，皮肤刺激性试验方法。
3、试验方法
3.1染毒方法：
普通级新西兰兔4只，雌雄各半。试验前将实验动物背部脊柱两侧被毛剪掉，去毛范围左、右各约3cm*3cm。取受试物约0.5ml涂抹在动物左侧皮肤上，涂抹面积约2.5cm*2.5cm，每天涂抹1次，连续涂抹14天，另一侧作空白对照。从第二天开始，每次涂抹前剪毛，用纯净水清除残留受试物，对照区作同样处理。一小时观察结果。试验结果如下表1所示。
表1本发明实施例1-3的产品对新西兰兔多次皮肤刺激性试验结果
Figure PCTCN2019080353-appb-000001
上述表1的结果显示：受试物对新西兰兔多次皮肤刺激性为无刺激性。
3、检测结果：在观察期内受试新西兰兔皮肤均未出现红斑和水肿的皮肤刺激反应，样品组每天每只动物积分值均为0分(实施例1的产品对新西兰兔多次皮肤刺激性试验结果见下表1所示)。
4、结果评价：依据《化妆品安全技术规范》2015年版，皮肤刺激性判断标准，本发明实施例1-3送检的产品经过多次皮肤几次强度均为无刺激性。
效果试验例2(增泡稳泡作用)
测试方法：
1)取5克待测表面活性剂、本发明所涉及的蚕丝水解液用纯净水稀释成5％的溶液，取溶液20ml，用同等力度相同时间震荡，测量震荡后的泡沫高度，目测泡沫密实度。并放置4小时，观察泡沫残余量；
2)以2.5克待测表面活性剂与2.5克本发明所涉及的蚕丝蛋白水解液，加纯净水至100ml，取溶液20ml。用同等力度相同时间震荡，测量震荡后的泡沫高度，目测泡沫密实度， 并放置6小时，观察泡沫残余量。
结果发现：相比没有复配的溶液，与本发明所涉及的蚕丝水解液复配的溶液，通过等力等时长震荡后，所获得的泡沫量有所增多，泡沫的密实度有明显加强，且放置6小时后的泡沫残余量与单独使用表面活性剂的4小时后的泡沫残余量相当或更多。
如图2所示，在同一浓度，同一体积，同一震荡力度下，复配性测试结论：本发明所涉及的蚕丝水解液在与其他表面活性剂复配时，具有很好的增泡、稳泡作用。
效果试验例3(抑菌试验)
通过测试，我们发现采用本发明的蚕丝蛋白水解工艺所获得的蚕丝蛋白水解液对糠秕马拉色菌具有一定的抑制作用。
如下表2所示，发现3％、4％这两种不同浓度的采用本发明所描述的蚕丝蛋白水解工艺所获得蚕丝蛋白水解液，分别对糠秕马拉色菌具有14％与24％的抑制率。
检测单位：广东省微生物分析检测中心
表2蚕丝蛋白水解液对糠秕马拉色菌的抑制作用
Figure PCTCN2019080353-appb-000002
我们通过采用不同浓度的蚕丝水解液测试其对大家所公认的影响头皮屑的主要微生物糠秕马拉色菌的抑制作用，发现3％、4％这两种不同浓度的采用本发明所描述的蚕丝蛋白水解工艺所获得蚕丝蛋白水解液，分别对糠秕马拉色菌具有14％与24％的抑制率。
另外，从以下多次试验的结果可以看出，用不加任何去屑止痒成分的配方所调制出的洗发水，同样具有去屑止痒效果，而且，干净的头皮还可以维持3-4天。由此可以得出一个结论：头皮屑的产生，跟头皮干燥与头皮养护具有直接关系。
在实际的生产配方中，因为要照顾到市场的普遍性，如果再在配方中配合适当的中草药类的杀菌剂或合成杀菌剂，解决微生物过量繁殖引起的头屑问题，两种机理同时应用，将会对抑制头皮屑的产生更好地起到协同增效效果。
本发明去屑止痒洗发养发组合物的技术方案优点是，通过只加蚕丝水解液的验证配方，验证了不加去屑止痒的杀菌剂，也可以使产品达到去屑止痒效果的事实，这在现有该类产品中是没有过的。
以下所有原料组份均为市售产品。
其中，原料组份中的去离子水为溶剂；乙二胺四乙酸二钠为金属螯合剂稳定体系；柠檬酸系PH值调节剂；甘油普通保湿剂；AESA表面活性剂为主发泡剂；咪唑啉为增泡剂；烯烃磺酸钠为增泡稳泡剂；二乙醇酰胺为增泡稳泡剂；醋酸丁酸纤维素为增稠稳定剂；蚕丝水解液为保湿调理剂可以通过增强头皮的保湿性而改善头皮的微生态环境，从而达到抑制头皮屑生成的目的；卡松为防腐剂；香精为赋香剂；氯化钠为增稠稳定剂。
本发明在配方中加入了采用本发明所述生产工艺获得的蚕丝水解液，该蚕丝水解液的主要特征是，其中的蚕丝水解蛋白的分子大部分集中在2万-20万道尔顿范围内，属于中小分子的蛋白质。
实施例4(去屑止痒洗发养发组合物的制备工艺)
一种含蚕丝蛋白成分的去屑止痒洗发养发组合物，包含以下重量比的组分：
去离子水78克、乙二胺四乙酸二钠0.1克、柠檬酸0.2克、甘油2克、AESA表面活性剂克10克、咪唑啉2克、烯烃磺酸钠1克、二乙醇酰胺1克、醋酸丁酸纤维素2克、实施例1的蚕丝水解液5克、卡松0.1克、香精0.1克、氯化钠适量；
制作时，将上述组分的原料在室温下混合，先将水、乙二胺四乙酸二钠加入锅中搅拌，溶解；依次加入AESA、咪唑啉、烯烃磺酸钠、二乙醇酰胺、甘油、醋酸丁酸纤维素溶解完全透明；再依次加入卡松、香精溶解完全透明；最后加入蚕丝水解液丝，搅拌均匀，加入盐调节好粘度(25℃)：5000，加入柠檬酸调节PH值5.8-6.5即可。
实施例5(去屑止痒洗发养发组合物的制备工艺)
一种含蚕丝蛋白成分的去屑止痒洗发养发组合物，包含以下重量比的组分：
去离子水85克、乙二胺四乙酸二钠(EDTA-2Na)0.1克、柠檬酸0.2克、甘油3克、AESA表面活性剂克15克、咪唑啉3克、烯烃磺酸钠(AOS)3克、二乙醇酰胺(6501)3克、醋酸丁酸纤维素(CAB)3克、实施例2的蚕丝水解液7克、卡松0.1克、香精0.1克、氯化钠适量。
制作时，将上述组分的原料在室温下混合，先将水、乙二胺四乙酸二钠加入锅中搅拌，溶解；依次加入AESA、咪唑啉、烯烃磺酸钠、二乙醇酰胺、甘油、醋酸丁酸纤维素溶解完全透明；再依次加入卡松、香精溶解完全透明；最后加入蚕丝水解液丝，搅拌均匀，加入盐调节好粘度(25℃)：5000，加入柠檬酸调节PH值5.8-6.5即可。
实施例6(去屑止痒洗发养发组合物的制备工艺)
一种含蚕丝蛋白成分的去屑止痒洗发养发组合物，包含以下重量比的组分：
去离子水82克、乙二胺四乙酸二钠0.1克、柠檬酸0.2克、甘油1.5克、AESA表面活性剂克12克、咪唑啉1克、烯烃磺酸钠2.5克、二乙醇酰胺2克、醋酸丁酸纤维素4克、实施例3的蚕丝水解液8克、卡松0.1克、香精0.1克、氯化钠适量；
制作时，将上述组分的原料在室温下混合，先将水、乙二胺四乙酸二钠加入锅中搅拌，溶解；依次加入AESA、咪唑啉、烯烃磺酸钠、二乙醇酰胺、甘油、醋酸丁酸纤维素溶解完全透明；再依次加入卡松、香精溶解完全透明；最后加入蚕丝水解液丝，搅拌均匀，加入盐调节好粘度(25℃)：5000，加入柠檬酸调节PH值5.8-6.5即可。
本发明在配方中加入了蚕丝水解液，属于滞留型，不易轻易冲洗的皮肤保湿成分，利用蚕丝主要的两种成分丝胶与丝素的作用，其中丝胶主要为胶原蛋白，丝素为角蛋白，蚕丝中所含有的18种氨基酸，其中人体所必需的或半必需的氨基酸10种均包含在丝胶与丝素中，通过只加蚕丝水解液的验证配方，验证了不加去屑止痒的杀菌剂，也可以使产品达到去屑止痒效果的事实。
本发明实施例的配方中，可加入现有市场上销售的任何洗发水混合而成；也可以在本发明的配方中加入适当的中草药类的杀菌剂或合成杀菌剂，解决微生物过量繁殖引起的头屑问题，两种机理同时应用，对更好地抑制头皮屑的产生起到协同增效的效果。
以下为去屑止痒洗发养发组合物的效果试验例内容。
效果试验例4
对本发明实施例4-6的去屑止痒洗发养发组合物进行微生物、卫生化学的检测项目，依据《化妆品安全技术规范》2015年版。
检测结果显示：根据《化妆品安全技术规范》2015年版对送检的三份样品(实施例4-6的产品)进行了卫生安全性检验，如下：
1、微生物检验：菌落总数、霉菌和酵母菌总数、耐热大肠菌群、金黄色葡萄球菌、铜绿假单胞菌检测结果均符合要求；
2、卫生化学检验：汞、砷、镉和去屑剂(包括水杨酸、酮康唑、氯咪巴唑、吡硫鎓锌、 吡罗克酮乙醇胺盐)检测结果均符合要求。
表3卫生化学检验结果
Figure PCTCN2019080353-appb-000003
表4的结论：卫生化学检验结果(不含铅汞砷、不含去屑剂)
表4微生物检验结果
检验项目 检验结果 限值
菌落总数(CFT/g) <10 ≤1000
霉菌和酵母菌总数(CFT/g) <10 ≤100
耐热大肠菌群/g 未检出 不得检出
金黄色葡萄球菌/g 未检出 不得检出
铜绿假单胞菌/g 未检出 不得检出
表4的结论：菌落总数均符合要求，并未检出任何细菌感染。
效果试验例5
为达到试验效果，经选择100名出现头皮屑、头皮瘙痒症状的志愿者予以测试，使用20天，每3天用实施例4-6的洗发液适量，进行清洗，按照正常的洗发步骤使用即可，经验证，有效率达98.6％。
蚕丝去屑洗发护发组合物的去屑效果测试效果，如下表5所示。
其中，发质类型分为油性、干性、中性和受损发；以下分别介绍。
油性：头发油腻，触摸有粘腻感，头皮屑多，缺乏光泽；
干性：头发干燥，触摸有粗糙感，不润滑，缺乏光泽，造型后易变性；
中性：头发光泽、柔顺、健康的发质；既不油腻也不干燥，软硬适度，丰润柔软，有自然的关泽；
受损发：头发干燥，触摸有粗糙感，缺乏光泽，颜色枯黄。
表5实施例4-6的蚕丝蛋白去屑洗发护发组合物去屑效果测试
Figure PCTCN2019080353-appb-000004
去屑效果说明：
①非常好：洗后头皮干净，看不见头屑，且能维持2-3天时间；②效果一般：洗后头皮干净、看不见头屑，但第二天又可见头屑；③没效果：洗后待头发干后可见头屑。
另外，如图3所示，本发明的验证配方所调制的样板，任意挑选12名志愿者使用，对头皮屑、头皮瘙痒均有一定程度的改善。
本发明以如何维护头皮微生态环境的理论为基础，通过提高皮肤保湿性能，改善头皮由生理脂质、天然保湿因子、头皮微生物种群所组成的头皮微生态环境，维护头皮健康，而达到去屑止痒的效果。
从多次试验的结果可以看出，用不加任何去屑止痒成分的配方所调制出的洗发水，同样具有去屑止痒效果，而且，干净的头皮还可以维持3-4天，具有配方简单，使用效果良好的特点。
以上所述，仅是本发明的较佳实施例而已，并非对本发明做任何形式上的限制，故凡未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。

Claims (9)

  1. 一种蚕丝蛋白水解液的制备方法，其特征在于，包括以下步骤：
    1)选择个大壳厚的优质种蚕的蚕茧并去除蚕茧中的蚕蛹、蚕衣与杂质，绞碎备用；
    2)使用0.1-1％的碳酸钠或碳酸氢钠溶液作为脱胶剂，其茧量为0.4-10％，水解温度控制在50-100℃水浴温度下脱胶2-4h，过滤得到水解蚕丝胶蛋白(滤液)和丝素蛋白纤维(滤渣)；所得滤液通过电渗析装置脱盐，得到的脱盐水解蚕丝胶蛋白留用，所脱出的盐溶液，可以用于下一次水解；
    3)将丝素蛋白纤维滤渣溶解在质量比浓度为30-50％的中性盐溶液中，温度为80-100℃；水解终点通过紫外可见分光光度计比较测试水解液的透光率来判定；
    4)将水解好的丝素蛋白液进行电透析，除掉溶液中的杂离子，循环至溶液的电导率为100-500us/cm，得到浅黄色丝蛋白纯溶液；分离出的电解质溶液可以用于下一次水解生产用；
    5)最后将质量浓度为1-5％的丝素蛋白液和1-5％的丝胶蛋白液混合，获得蛋白质分子量为2万-20万道尔顿的全蚕丝水解液。
  2. 根据权利要求1所述的蚕丝蛋白水解液的制备方法，其特征在于：步骤1)中，所述蚕茧的培育方法为：
    1)桑田的选择：
    选择阳光充足、昼夜温差大的云南山区种植桑树，桑叶含糖量高，有利于蚕宝宝的健康成长，从而获得壳厚个大的优质茧壳，另外，云南山区独特的小盆地结构，形成了一个天然的屏障，从而减少非养蚕区的农药飘散到养蚕区，从而对终产物的农药残留有保障；
    2)种蚕的精选：
    种蚕是从蚕业技术站获得的二代蚕，采用种蚕是为了所获得的蚕丝胶蛋白与丝素蛋白的含量稳定，从而获得水解蚕丝胶蛋白与水解丝素蛋白比较稳定比例的水解终产品；
    3)养殖环境：
    桑蚕的养殖环境于后期产品的微生物控制以及蚕叶病相关；所述桑蚕的养殖环境是采用无菌、通风、干燥的蚕室内养殖，以降低最终产品的病菌、微生物等风险；
    4)储存条件：
    蚕丝是活性蛋白，需要在阴凉、干燥、通风处储存。
  3. 根据权利要求1所述的蚕丝蛋白水解液的制备方法，其特征在于：步骤3)中，所述中性盐溶液选自质量比浓度为30-50％的无水CaCl 2、CaCl 2-H 2O、CaCl 2-2H 2O或LiBr溶液。
  4. 根据权利要求1所述的蚕丝蛋白水解液的制备方法，其特征在于：步骤3)中，所述 对水解终点的控制，是保证步骤5)所获得的终产物的蚕丝蛋白的分子量控制在2万-20万道尔顿的区间范围，主要集中在10万-20万道尔顿区间范围。
  5. 一种含蚕丝蛋白成分的去屑止痒洗发养发组合物，其特征在于：包括以下重量百分比的组分：
    去离子水70-85份、乙二胺四乙酸二钠0.1-03份、柠檬酸0.2-0.4份、甘油1-3份、AESA表面活性剂10-15份、咪唑啉1-3份、烯烃磺酸钠1-3份、二乙醇酰胺1-3份、醋酸丁酸纤维素2-4份、蚕丝蛋白水解液1-8份、卡松0.1-0.3份、香精0.1-0.3份、氯化钠适量。
  6. 权利要求5所述的含蚕丝蛋白成分的去屑止痒洗发养发组合物，其特征在于：所述蚕丝蛋白水解液是通过以下工艺制备得到：
    1)按照常规方法，使用弱碱性水溶液作为脱胶剂对蚕茧脱胶，在脱胶剂溶液质量百分数为0.4-6％，pH为8-11，水解温度为50-100℃的条件下对蚕茧脱胶；
    2)过滤步骤1)的溶液，形成脱胶水解液和蚕丝丝素纤维；
    3)将步骤2)滤出的脱胶水解液通过电渗析后分成丝胶水解液和渗析离子溶液，将丝胶水解液留住，渗析离子溶液将转入下一次丝胶水解用；水解终点通过紫外可见分光光度计比较测试水解液的透光率来判定；
    4)将步骤2)滤得的蚕丝丝素纤维溶解在温度为60-100℃，质量百分数为30-60％的中性盐溶液中，形成蚕丝丝素蛋白液；
    5)将步骤4)水解好的蚕丝丝素蛋白液进行电透析除掉溶液中的离子，循环至溶液的电导率降至100-500us/cm，得到浅黄色蚕丝蛋白纯溶液，电透析后的离子溶液可循环作为步骤4)中的中性溶液使用；
    6)将步骤3)的丝胶水解液和步骤5)的蚕丝蛋白纯溶液混合均匀，即制得具有表面活性剂特性的新型蚕丝蛋白质水解液。
  7. 根据权利要求4所述的含蚕丝蛋白成分的去屑止痒洗发养发组合物，其特征在于：
    步骤1)中，所述脱胶剂采用碳酸钠或碳酸氢钠水溶液；所述水解温度为50-80℃，时间为2-4小时；
    步骤4)所述中性盐溶液为CaCl 2、CaCl 2-H 2O、CaCl 2-2H 2O或者LiBr溶液。
  8. 权利要求4-7中任一项所述的含蚕丝蛋白成分的去屑止痒洗发养发组合物的制备方法，其特征在于：其制作工艺为：
    1)将上述组分的原料在室温下混合，先将水、乙二胺四乙酸二钠加入锅中搅拌，溶解；
    2)依次加入AESA、咪唑啉、烯烃磺酸钠、二乙醇酰胺、甘油、醋酸丁酸纤维素溶解完全透明；
    3)依次加入卡松、香精溶解完全透明；
    4)最后，加入蚕丝水解液丝，搅拌均匀，加入盐调节好粘度(25℃)：5000，加入柠檬酸调节PH值5.8-6.5即可。
  9. 一种头皮去屑止痒的方法，在洗发时，所使用的去屑止痒洗发养发组合物是采用权利要求6所述的含蚕丝蛋白成分的去屑止痒洗发养发组合物的制备方法所制备得到的去屑止痒洗发养发组合物，其具有改善头皮的生理脂质、天然保湿因子、头皮微生物种群所组成的头皮微生态环境。
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