CN110613627A - Cosmetic and preparation method thereof - Google Patents

Abstract

The invention relates to the field of washing and caring products, and particularly provides a cosmetic and a preparation method thereof. The cosmetic comprises 0.5-5 wt% of timosaponin enzymatic hydrolysate and/or timosaponin AIII. The cosmetic can effectively remove dandruff and reduce scalp itch, has high safety, does not damage hair and scalp surface structure, is beneficial to keeping scalp self balance, has no side effect after long-term use, and does not aggravate dandruff breeding.

Description

Cosmetic and preparation method thereof

Technical Field

The invention relates to the field of washing and caring products, and particularly relates to a cosmetic and a preparation method thereof.

Background

It is statistical that more than 80% of adults suffer from dandruff to varying degrees, and the dandruff is developed by many reasons, such as metabolites of fungi (mainly malassezia), improper combing, improper hair care causing inflammation, accelerated proliferation of skin cells, and exfoliation of dead skin, so-called dandruff. In response to consumer needs, there are currently a large number of anti-dandruff shampoo products on the market. However, the traditional dandruff removing method mainly uses chemical dandruff removing agents such as salicylic acid, zinc pyrithione (also called zinc pyrithione), piroctone olamine and the like, and the chemical components are easy to damage the structure of the epidermis, disturb the balance of the epidermis and aggravate the growth of dandruff after long-term use.

In view of the above, the present invention is particularly proposed.

Disclosure of Invention

The first object of the present invention is to provide a cosmetic which can effectively remove dandruff and reduce scalp itching, is highly safe, does not damage the hair and the surface structure of the scalp, is advantageous for maintaining the scalp self-balance, has no side effects after long-term use, and does not aggravate dandruff breeding.

The second purpose of the invention is to provide a preparation method of the cosmetic.

In order to achieve the above purpose of the present invention, the following technical solutions are adopted:

in a first aspect, the invention provides a cosmetic, which comprises an timosaponin enzymatic hydrolysate and/or timosaponin AIII, wherein the weight percentage content of the timosaponin enzymatic hydrolysate and/or timosaponin AIII is 0.5-5%;

preferably, the cosmetic comprises a shampoo, a conditioner or a hand sanitizer.

As a further preferred technical scheme, the timosaponin enzymatic hydrolysate and/or timosaponin AIII is/are 1-5% by weight;

preferably, the shampoo further comprises at least one of sodium laureth sulfate, cocamidopropyl betaine, or sodium lauroamphoacetate;

preferably, the sodium laureth sulfate is present in an amount of 9% to 13%, preferably 9.5% to 11%, by weight;

preferably, the weight percentage content of cocamidopropyl betaine is 4% to 9%, preferably 5% to 8%;

preferably, the weight percentage content of the sodium lauroamphoacetate is 1 to 5 percent, and preferably 2 to 4 percent;

preferably, the shampoo comprises the following components in percentage by weight: 9-13% of sodium laureth sulfate, 4-9% of cocamidopropyl betaine, 1-5% of sodium lauroamphoacetate, 0.5-5% of timosaponin enzymolysis conversion product and/or timosaponin AIII and the balance of water;

preferably, the shampoo comprises the following components in percentage by weight: 9.5-11% of sodium laureth sulfate, 5-8% of cocamidopropyl betaine, 2-4% of sodium lauroamphoacetate, 1-5% of timosaponin enzymolysis conversion product and/or timosaponin AIII and the balance of water.

As a further preferred technical scheme, the shampoo further comprises at least one of a softener, a humectant or a chelating agent;

preferably, the shampoo further comprises at least one of a thickener, a preservative or a fragrance.

As a further preferred technical scheme, the softener comprises polyquaternium and/or guar gum hydroxypropyl trimethyl ammonium chloride;

preferably, the polyquaternium comprises polyquaternium-7 and/or polyquaternium-10;

preferably, the weight percentage content of the polyquaternium is 0.5 to 2.5 percent;

preferably, the weight percentage content of the guar gum hydroxypropyl trimethyl ammonium chloride is 0.1-0.9%;

preferably, the humectant comprises trimethylolpropane tricaprylate;

preferably, the weight percentage content of the trimethylolpropane tricaprylate is 0.1-0.6%;

preferably, the chelating agent comprises an organic acid and/or an ethylenediaminetetraacetic acid derivative;

preferably, the organic acid comprises citric acid and/or tartaric acid;

preferably, the weight percentage content of the organic acid is 0.2 to 0.7 percent;

preferably, the ethylenediaminetetraacetic acid derivatives include ethylenediaminetetraacetic acid sodium salt;

preferably, the sodium salt of ethylenediaminetetraacetic acid comprises disodium ethylenediaminetetraacetate and/or tetrasodium ethylenediaminetetraacetate;

preferably, the weight percentage content of the ethylene diamine tetraacetic acid derivative is 0.1% -0.5%;

preferably, the weight percentage content of the thickening agent is 0.1% -0.4%;

preferably, the preservative is present in an amount of 0.1% to 0.3% by weight;

preferably, the essence accounts for 0.5 to 5 weight percent.

In a second aspect, the present invention provides a method for preparing the above cosmetic, comprising: mixing the above components uniformly to obtain the cosmetic.

As a further preferred embodiment, the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, optional polyquaternary ammonium salt and optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with optional trimethylolpropane tricaprylate and optional organic acid, and then mixing with the rest components;

preferably, the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, an optional polyquaternary ammonium salt and an optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with an optional trimethylolpropane tricaprylate and an optional organic acid, mixing with water and an optional ethylene diamine tetraacetic acid derivative, and finally mixing with the rest components;

preferably, the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, optional polyquaternary ammonium salt and optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with optional trimethylolpropane tricaprylate and optional organic acid, mixing with water and optional ethylene diamine tetraacetic acid derivatives, mixing with optional thickening agent, optional preservative and optional essence, and finally mixing with timosaponin enzymatic conversion product and/or timosaponin AIII.

As a further preferred technical scheme, the mixing temperature of sodium laureth sulfate, sodium lauroamphoacetate, an optional polyquaternium salt and an optional guar gum hydroxypropyl trimethyl ammonium chloride is 60-70 ℃, and/or the mixing time is 10-20 min;

preferably, the mixing temperature when mixing with the optional trimethylolpropane tricaprylate and the optional organic acid is 75-85 ℃, and/or the mixing time is 15-30 min;

preferably, the mixing temperature when mixing with water and optionally the ethylenediaminetetraacetic acid derivative is 75-85 ℃ and/or the mixing time is 5-10 min;

preferably, the mixing temperature when mixing with the optional thickener, optional preservative and optional perfume is 35-45 ℃;

preferably, the mixing temperature when the timosaponin enzymatic hydrolysate and/or timosaponin AIII are mixed is 35-45 ℃;

preferably, the mixing means comprises stirring;

preferably; the stirring speed was 800-1000 rpm.

As a further preferred technical scheme, before the timosaponin enzymatic hydrolysate is mixed with the rest components, the method also comprises the step of preparing a timosaponin enzymatic hydrolysate into timosaponin enzymatic hydrolysate suspension, and then mixing the timosaponin enzymatic hydrolysate suspension with the rest components;

preferably, the method further comprises the step of preparing timosaponin AIII into timosaponin AIII suspension or timosaponin AIII nanoliposome before mixing timosaponin AIII with the rest of the components, and then mixing with the rest of the components.

As a further preferred technical scheme, the timosaponin enzymatic hydrolysate suspension is prepared by adopting the following method: ultrasonically dispersing the timosaponin enzymatic hydrolysate to obtain timosaponin enzymatic hydrolysate suspension;

preferably, the timosaponin AIII suspension is prepared by the following method: ultrasonically dispersing timosaponin AIII to obtain timosaponin AIII suspension;

preferably, the ultrasonic dispersion time is 8-12 min;

preferably, the solvent used for ultrasonic dispersion comprises water;

preferably, the weight ratio of the timosaponin enzymolysis conversion product or timosaponin AIII to the solvent used for ultrasonic dispersion is 1: (0.5-1.5).

As a further preferred technical scheme, the timosaponin AIII nano-liposome is prepared by adopting the following method: mixing the timosaponin AIII solution with the membrane material solution, and removing the solvent and water to obtain a lipid membrane; then sequentially hydrating and homogenizing the lipid film to obtain timosaponin AIII nano-liposome;

preferably, the means of homogenization comprises high pressure homogenization;

preferably, the high-pressure homogenization condition comprises that circulation is carried out for 2-6 times under the condition of 10000-30000 PSI;

preferably, the membrane material comprises at least one of phospholipid, distearoylphosphatidylethanolamine-polyethylene glycol or distearoylphosphatidylacetamide-methoxypolyethylene glycol.

Compared with the prior art, the invention has the beneficial effects that:

the cosmetic provided by the invention comprises the timosaponin enzymatic hydrolysis converted substance and/or timosaponin AIII with specific content, and the timosaponin enzymatic hydrolysis converted substance or timosaponin AIII has obvious improvement effect on the problems of scalp itch, excessive scurf and the like caused by fungi such as malassezia and the like, has high safety, does not have side effect after long-term use, does not aggravate scurf breeding, can effectively remove scurf and reduce scalp itch, has high safety, does not damage the hair and scalp surface layer structure, is favorable for keeping scalp self balance, does not have side effect after long-term use, and does not aggravate scurf breeding. If the content of the timosaponin enzymatic hydrolysate and/or timosaponin AIII is too low, the effect of removing dandruff and relieving itching is poor, the content is too high, the effect of removing dandruff and relieving itching cannot be further improved, and the cost is increased.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.

Studies on in vitro marasmius resistance of timosaponin enzymolysis conversion product and timosaponin AIII

The inventor carries out the research of the action of resisting malassezia in vitro on the timosaponin enzymolysis conversion product and timosaponin AIII:

1 materials and methods

1.1 Experimental materials: timosaponin enzymolysis product, timosaponin AIII.

1.2 strains: 1) standard strains: malassezia furfur BNCC No: BNCC337308 (supplied by North Nawa Biotechnology Ltd., Suzhou). 2) Malassezia clinical isolates: malassezia globosa 4 strain, malassezia furfur 2 strain.

1.3 Medium

Safburg weak medium with olive oil: 1% peptone, 1.8% agar, 4% glucose, 0.01% yeast extract, 0.25% glyceryl monostearate, 0.2% tween-80, 0.005% chloramphenicol, 0.05% cycloheximide and 4% olive oil.

Liquid culture medium of malassezia: 20g/L glucose, 4g/L taurocholate, 1ml/L glycerol, 0.5g/L glyceryl monostearate, 200.4 ml/L Tween-and RPMI 164010.4 g/L.

1.4 preparation of the liquid medicine

Weighing appropriate amount of ketoconazole and fluconazole, and preparing 5120mg/L medicament stock solution by using sterilized distilled water under the aseptic condition. Taking a proper amount of ketoconazole, fluconazole, timosaponin enzymatic hydrolysis conversion products and timosaponin A III, respectively fully dissolving with dimethyl sulfoxide (DMSO), diluting with sterile distilled water to obtain a medicament stock solution with a concentration of 1280mg/L (the concentration of DMSO in the final volume is less than or equal to 2%), sealing, and storing at-80 ℃ for later use. When in use, the stock solution is taken out and frozen, and then diluted into solutions with the concentration of 128, 64, 32, 16, 8, 4 and 2mg/L respectively by using a malassezia liquid culture medium for drug sensitivity experiments.

1.5 preparation of the bacterial suspension

Continuously subculturing the tested strain on Sabouraud weak culture medium containing olive oil for 2 times, subculturing at 2 nd 32 deg.C for 5d, collecting two colonies with diameter of 1mm or more, preparing into bacterial suspension with 1mL sterile physiological saline, oscillating for 15s, adjusting to 0.5 McLeod unit with McLeod turbidimeter, counting on blood cell counting plate to 2 × 10⁹CFU/L, then diluting the bacterial suspension to 2X 10 concentration by using malassezia liquid culture medium⁶CFU/L (diluted 1000 times) of bacterial suspension is ready for use.

1.6 drug susceptibility test

Single drug allergy: in vitro drug susceptibility testing was performed on malassezia by yeast microdilution according to the protocol M27-A2 established by the national institute for clinical laboratory standardization (NCCLS). And taking a 96-hole microplate, and adding 100 mu L of bacterial liquid into each hole of 1-11 rows of each row. Adding 80 mu L of a liquid medicine with a multiple concentration into each hole from the 1 st to the 10 th holes from high to low, taking the 11 th hole as a growth control (positive control), and adding 80 mu L of a malassezia liquid culture solution into each hole; column 12 is a sterility control (negative control) and 180. mu.L of Malassezia liquid medium is added, 20. mu.L of Almaran blue is added to each well.

1.7 cultivation and result determination

And (3) incubating the inoculated drug sensitive culture plate in a wet box at 32 ℃, observing the result after culturing for 24h, and taking a test hole with the lowest drug concentration, in which fungi are completely inhibited (do not grow), to obtain the Minimum Inhibitory Concentration (MIC) of the drug. Each drug was given 3 rows simultaneously and the results averaged over 3 numbers. The whole drug sensitization process is repeated for 2 times.

The results of bacteriostatic experiments show that the MIC of timosaponin AIII to 2 kinds of fungi reaches 8 mg.L^-1(see table 1), the timosaponin zymolysis conversion product has better bacteriostatic activity on 2 fungi, and the MIC reaches 4 mg.L^-1The effect is even better than that of ketoconazole. Although the MIC of the timosaponin enzymatic hydrolysate is lower than that of fluconazole, the timosaponin enzymatic hydrolysate has a wide prospect in being used in anti-dandruff lotions in view of certain irritation of fluconazole in dandruff treatment.

TABLE 1 in vitro antibacterial Activity (MIC, mg/L) of different drugs

Based on the research results, according to one aspect of the invention, a cosmetic is provided, which comprises 0.5-5 wt% of timosaponin enzymolysis conversion product and/or timosaponin AIII.

The cosmetic comprises an anemarrhena saponin enzymatic hydrolysis converted substance and/or an anemarrhena saponin AIII with specific content, and the anemarrhena saponin enzymatic hydrolysis converted substance or the anemarrhena saponin AIII has obvious improvement effect on the problems of scalp itch, excessive scurf and the like caused by fungi such as malassezia and the like, and has high safety, no side effect is caused after long-term use, and the scurf cannot be aggravated to breed, so that the cosmetic can effectively remove the scurf, reduce the scalp itch, has high safety, cannot damage the surface structures of hair and scalp, is favorable for keeping the self balance of the scalp, has no side effect after long-term use, and cannot aggravate the scurf. If the content of the timosaponin enzymatic hydrolysate and/or timosaponin AIII is too low, the effect of removing dandruff and relieving itching is poor, the content is too high, the effect of removing dandruff and relieving itching cannot be further improved, and the cost is increased.

The rhizoma anemarrhenae saponin enzymolysis conversion product is obtained by performing enzymolysis conversion on rhizoma anemarrhenae extract with enzyme, and contains active ingredients such as timosaponin AIII and timosaponin BII. Researches show that the timosaponin enzymatic hydrolysate or timosaponin AIII has an inhibiting effect on malassezia furfur and malassezia globosa, has a similar effect to that of the existing bacteriostatics ketoconazole and fluconazole, has a good bacteriostatic activity, wherein the MIC (Minimum Inhibitory Concentration) value is between 2 and 16mg/L, and has an obvious improvement effect on the problems of scalp pruritus and excessive scurf caused by fungi such as malassezia and the like. Moreover, the timosaponin enzymolysis conversion product and the timosaponin AIII are both derived from natural plant rhizoma anemarrhenae and are not synthesized chemical products, so that the timosaponin enzymolysis conversion product has higher safety, cannot damage the scalp structure, cannot disturb the self balance of the epidermis, and has no side effect after long-term use.

In the present invention, the weight percentage of timosaponin enzymatic hydrolysate and/or timosaponin aiii is typically, but not limited to, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%.

Preferably, the cosmetic comprises a shampoo, a conditioner or a hand sanitizer.

In a preferred embodiment, the timosaponin enzymatic hydrolysate and/or timosaponin aiii is present in an amount of 1% to 5% by weight. By further optimizing the content of timosaponin enzymolysis conversion product and/or timosaponin AIII, the cosmetic has better effects of removing dandruff and relieving itching.

In a preferred embodiment, the shampoo further comprises at least one of sodium laureth sulfate, cocamidopropyl betaine, or sodium lauroamphoacetate. The shampoo also comprises sodium laureth sulfate, cocamidopropyl betaine, sodium lauroamphoacetate, a combination of sodium laureth sulfate and cocamidopropyl betaine, a combination of cocamidopropyl betaine and sodium lauroamphoacetate, a combination of sodium laureth sulfate, sodium cocamidopropyl betaine and sodium lauroamphoacetate, or a combination of sodium laureth sulfate, sodium cocamidopropyl betaine and sodium lauroamphoacetate. When the shampoo also comprises the components, the shampoo has good decontamination and cleaning effects.

The sodium laureth sulfate is an anionic surfactant, has good detergency and diffusivity, is easy to generate a large amount of foam, and has antistatic property, smoothness, softness and strong detergency.

The cocamidopropyl betaine is an amphoteric surfactant, has excellent stability under acidic and alkaline conditions, good compatibility, small irritation, easy water solubility, stability to acid and alkali, more foam, strong detergency, excellent thickening property, softness, bactericidal property, antistatic property and hard water resistance.

Sodium lauroamphoacetate is an amphoteric surfactant, namely, a positive charge group and a negative charge group, is very mild, low in toxicity and low in irritation, can effectively reduce the irritation of other surfactants, and has very high foaming capacity, fine and stable foam, light color and low smell.

Preferably, the sodium laureth sulfate is present in an amount of 9% to 13%, preferably 9.5% to 11% by weight. The weight percent of sodium laureth sulfate is typically, but not limited to, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, or 13%.

Preferably, the weight percentage content of cocamidopropyl betaine is 4% to 9%, preferably 5% to 8%. The weight percent content of cocamidopropyl betaine is typically, but not limited to, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, or 9%.

Preferably, the weight percentage content of the sodium lauroamphoacetate is 1 to 5 percent, and preferably 2 to 4 percent. The weight percent content of sodium lauroamphoacetate is typically, but not limited to, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%.

In a preferred embodiment, the shampoo comprises the following components in percentage by weight: 9-13% of sodium laureth sulfate, 4-9% of cocamidopropyl betaine, 1-5% of sodium lauroamphoacetate, 0.5-5% of timosaponin enzymolysis conversion product and/or timosaponin AIII and the balance of water.

The "balance of water" refers to the difference between 100% by weight of water in the shampoo minus the sum of the weight percentages of the remaining components.

The shampoo comprises specific contents of sodium laureth sulfate, cocamidopropyl betaine, sodium lauroamphoacetate, timosaponin enzymolysis conversion products and/or timosaponin AIII, water and the like, wherein the sodium laureth sulfate is matched with the cocamidopropyl betaine, so that the shampoo has good washing and dirt removing capabilities and can effectively remove stains on hair and scalp; sodium lauroamphoacetate can reduce irritation of other surfactants, reduce irritation of shampoo to hair and scalp, prevent surface layer structure of hair and scalp from being damaged, and keep scalp self-balance; the converted product of timosaponin enzymolysis or timosaponin AIII has obvious improvement effect on scalp itching, excessive dandruff and other problems caused by malassezia and other fungi, and has high safety, no side effect after long-term use, and no aggravation of dandruff breeding. The components are scientifically matched, so that the shampoo can effectively remove dandruff and reduce scalp itching, and has good decontamination and cleaning effects.

In a preferred embodiment, the shampoo comprises the following components in percentage by weight: 9.5-11% of sodium laureth sulfate, 5-8% of cocamidopropyl betaine, 2-4% of sodium lauroamphoacetate, 1-5% of timosaponin enzymolysis conversion product and/or timosaponin AIII and the balance of water.

By further optimizing the content of the components, the components are more scientifically and reasonably matched, and the dandruff removing, itching relieving and cleaning effects of the shampoo can be further improved.

In a preferred embodiment, the shampoo further comprises at least one of a softener, a moisturizer, or a chelating agent; the shampoo may also include, for example, a softener, a moisturizer, a chelating agent, a combination of a softener and a moisturizer, a combination of a moisturizer and a chelating agent, a combination of a softener and a chelating agent, or a combination of a softener, a moisturizer and a chelating agent, and the like. The shampoo also comprises the components, so that the flexibility, the moisture retention and the low irritation of the shampoo can be effectively enhanced, and the quality of the shampoo is improved.

Preferably, the shampoo further comprises at least one of a thickener, a preservative or a fragrance. The shampoo, for example, further comprises a thickener, a preservative, a fragrance, a combination of a preservative and a fragrance, a combination of a thickener and a preservative, a combination of a thickener and a fragrance, or a combination of a thickener, a preservative and a fragrance. The shampoo also comprises the components, so that the antiseptic property of the shampoo can be effectively enhanced, the consistency, stability and fragrance of the shampoo can be adjusted, and the sensory quality such as the property, the smell and the like of the shampoo is better.

In a preferred embodiment, the softener comprises a polyquaternium and/or guar hydroxypropyltrimonium chloride. Softeners include, but are not limited to, polyquaternium, guar hydroxypropyltrimonium chloride, or a combination of polyquaternium and guar hydroxypropyltrimonium chloride.

The polyquaternium is made of polymers synthesized by grafting quaternized fatty alkyl on modified natural polymers (saccharides, cellulose and protein) or double-bond-containing cationic monomers, has a plurality of cationic positions in each molecule, has high relative molecular weight, and is firmly adsorbed on the surface with negative charge in the hair protein structure by the attraction of ionic static electricity, so that fatty hydrocarbon chains are retained on the surface of hair cuticle, wherein the fat part deposited on the hair surface has good conditioning effect, and the hair surface is smooth, lubricated, soft and easy to comb; the conductivity of quaternary ammonium salts reduces the build-up of static electricity on the hair, thereby reducing hair brushing and improving hair manageability.

Guar hydroxypropyltrimonium chloride, also known as guar gum, is a cationic polymer prepared by purifying natural guar and chemically modifying the guar, can provide good dry and wet hand feeling when used in shampoo, and is easy to wash and free from accumulation after being used for many times. Guar gum has direct conditioning effect on hair and skin, can increase adsorption of emulsified silicone oil on hair (by 2-5 times), maintain stable emulsification state of water-insoluble components such as emulsified silicone oil and pearling agent, resist static, and prevent excessive hair scattering.

Preferably, the polyquaternium comprises polyquaternium-7 and/or polyquaternium-10. Polyquaternium includes, but is not limited to, Polyquaternium-7, Polyquaternium-10, or a combination of Polyquaternium-7 and Polyquaternium-10. Polyquaternium-7 strengthens and stabilizes shampoo foam while imparting excellent lubricity, wet combability and shine to hair without excessive accumulation. The polyquaternium-10 is used for hair, has strong affinity, can repair hair splits, forms a transparent and continuous film on the hair, and also has good moisturizing performance and can improve the damaged hair quality.

Preferably, the weight percentage of the polyquaternium is 0.5 to 2.5 percent. The weight percent of the above-mentioned polyquaternium is typically, but not limited to, 0.5%, 0.6%, 0.8%, 1%, 1.2%, 1.4%, 1.5%, 1.6%, 1.8%, 2%, 2.2%, 2.4%, or 2.5%. When the content of the polyquaternium is within the above range, the conditioning effect on hair can be optimal, when the content is too high, the hair is too soft and is not easy to comb, and when the content is too low, the hair is easy to generate static electricity and is not easy to comb.

Preferably, the guar hydroxypropyltrimonium chloride is present in an amount of 0.1 to 0.9% by weight. The weight percent content of guar hydroxypropyltrimonium chloride is typically, but not limited to, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, or 0.9%. When the content of the guar gum hydroxypropyl trimethyl ammonium chloride is in the range, the conditioning effect on hair can be optimal, and the hair is smooth, not easy to scatter and easy to comb.

In a preferred embodiment, the humectant comprises trimethylolpropane tricaprylate. Trimethylolpropane tricaprylate is a colorless transparent liquid, is a novel efficient refreshing type moisturizing agent, can rapidly improve the moisture retention of skin and hair in personal care products, stimulates the cell activity, has the effects of keeping the skin moist, smooth and preventing dryness, and provides refreshing natural feeling.

Preferably, the trimethylolpropane tricaprylate is present in an amount of 0.1% to 0.6% by weight. The weight percent of trimethylolpropane tricaprylate is typically, but not limited to, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, or 0.6%. When the content of the trimethylolpropane tricaprylate is in the range, the shampoo has the best moisturizing effect, and can make hair more refreshing and natural; if the content is too low, the moisturizing effect is relatively poor; if the content is too high, the hair will not be refreshing and natural.

In a preferred embodiment, the chelating agent comprises an organic acid and/or an ethylenediaminetetraacetic acid derivative. Chelating agents include, but are not limited to, organic acids, derivatives of ethylenediaminetetraacetic acid, or combinations of organic acids and derivatives of ethylenediaminetetraacetic acid. The chelating agent can improve the clarity of shampoo, prevent or reduce deposition of calcium magnesium soap insoluble substance on hair during washing hair with hard water, and stabilize foam. The organic acid and/or the ethylene diamine tetraacetic acid derivative can form water-soluble double salt with trace metal ions to play a role in chelation, so that the transparency of the shampoo is improved, and the deposition of insoluble substances is avoided.

Preferably, the organic acid comprises citric acid and/or tartaric acid. Organic acids include, but are not limited to, citric acid, tartaric acid, or a combination of citric acid and tartaric acid.

The organic acid can play a role in chelation, and can enable the pH of the shampoo to be closer to the pH of a human body, so that the irritation of the shampoo is further reduced. The citric acid and the tartaric acid have wide sources, low price and relatively low acidity, can relatively mildly adjust the pH value of the shampoo, and have smaller irritation to skin and safer use.

Preferably, the weight percentage of the organic acid is 0.2% -0.7%. The weight percent content of organic acid is typically, but not limited to, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, or 0.7%. The content of the organic acid needs to be in a reasonable range, and the pH value of the shampoo cannot be matched with the pH value of a human body due to too high or too low organic acid content, so that the required pH adjusting effect cannot be achieved.

Preferably, the ethylenediaminetetraacetic acid derivative comprises ethylenediaminetetraacetic acid sodium salt. The ethylene diamine tetraacetic acid derivative refers to a salt formed by ethylene diamine tetraacetic acid and metal ions. The sodium salt of ethylene diamine tetraacetic acid has wide sources and wide coordination performance, is an important chelating agent, can form stable chelate with almost all metal ions, and can remove the metal ions adhered to hair and scalp.

Preferably, the sodium salt of ethylenediaminetetraacetic acid comprises disodium ethylenediaminetetraacetate and/or tetrasodium ethylenediaminetetraacetate. The sodium salts of ethylenediaminetetraacetic acid include, but are not limited to, disodium ethylenediaminetetraacetate, tetrasodium ethylenediaminetetraacetate, or a combination of disodium ethylenediaminetetraacetate and tetrasodium ethylenediaminetetraacetate.

Preferably, the weight percentage of the ethylene diamine tetraacetic acid derivative is 0.1% -0.5%. The weight percentage of the above-mentioned ethylenediaminetetraacetic acid derivative is typically, but not limited to, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, or 0.5%. When the content of the ethylenediaminetetraacetic acid derivative is within the range, the chelating effect on metal ions in water is good, when the content is too low, a good chelating effect cannot be realized, and when the content is too high, resources are wasted.

In a preferred embodiment, the thickener is present in an amount of 0.1% to 0.4% by weight. The weight percent of thickener is typically, but not limited to, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, or 0.4%.

Preferably, the preservative is present in an amount of 0.1% to 0.3% by weight. The preservative is typically, but not limited to, 0.1%, 0.15%, 0.2%, 0.25%, or 0.3% by weight.

Preferably, the essence accounts for 0.5 to 5 weight percent. The weight percent of perfume is typically, but not limited to, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%.

It is verified that when the content of the thickener, the preservative or the essence is in the above range, the viscosity, the stability, the shelf life or the fragrance of the obtained shampoo are in a better range, the sensory quality such as the property, the smell and the like of the shampoo is better, and the shape of the shampoo is deteriorated if the content is too high or too low, and the shelf life of the shampoo is not in a reasonable range.

It should be understood that the term "weight percent" of each component referred to in the present invention refers to the weight of the component as a percentage of the total weight of the cosmetic or shampoo.

The timosaponin enzymolysis conversion product or timosaponin AIII can be prepared by any one of the existing methods or by the existing preparation process.

For example, the preparation method of the timosaponin enzymatic hydrolysate comprises the following steps:

(1) preparing an ethanol extract of rhizoma anemarrhenae: weighing an appropriate amount of rhizoma anemarrhenae (decoction pieces), heating and refluxing for 2 times by 6 times of 50% ethanol, extracting for 2h each time, mixing the extractive solutions, performing rotary evaporation under reduced pressure to recover ethanol, and concentrating to a concentration of 1.5g medicinal material/mL extractive solution to obtain timosaponin ethanol extract.

(2) Preparing an enzymolysis conversion product of timosaponin: weighing an ethanol extract of rhizoma anemarrhenae, adding 1-2 times of beta-glucosidase (50U/mg), placing in a conical flask with a plug, adding an appropriate amount of acetic acid-sodium acetate buffer solution with the pH value of 4.0, shaking, incubating for 2h, and drying to obtain an enzymolysis conversion product I of timosaponin. The timosaponin A III content in the enzymatic hydrolysate I is 40-55%.

(3) Purifying the timosaponin enzymatic hydrolysate: and (3) adding an alkaline aqueous solution (ammonia water or NaOH) to wash the enzymatic hydrolysis converted substance before drying, centrifuging, taking the precipitate, and drying to obtain the timosaponin enzymatic hydrolysis converted substance II. The timosaponin AIII in the converted product has timosaponin AIII content of about 55-65%.

The purification method can be any one of the following two methods:

the method comprises the following steps: ammonia water washing and purification: taking out after enzymolysis, mixing, centrifuging at 3000r/min for 10min, and discarding supernatant. Adding 200ml ammonia solution into the precipitate, stirring for 10min, mixing, centrifuging at 3000r/min for 10min, removing supernatant, and collecting precipitate. Drying and collecting to obtain the timosaponin enzymatic hydrolysate II-1.

The second method comprises the following steps: washing and purifying with NaOH solution: after the enzymolysis is finished, taking 200ml of the enzymolysis liquid, adding 80ml of 1% NaOH solution (taking 1g of NaOH solid, adding distilled water to 100ml, and obtaining the product), mixing uniformly, centrifuging at the rotating speed of 3000r/min for 10min, removing supernatant, and taking precipitate. Drying and collecting to obtain the timosaponin enzymatic hydrolysate II-2.

According to another aspect of the present invention, there is provided a method for preparing the above cosmetic, comprising: mixing the above components uniformly to obtain the cosmetic. The method has simple process and low preparation cost, and can obtain cosmetic with good decontamination, dandruff removing and itching relieving effects, high safety, no side effect, and no aggravation of dandruff breeding.

In a preferred embodiment, the mixing comprises: sodium laureth sulfate, sodium lauroamphoacetate, optionally a polyquaternium salt and optionally guar hydroxypropyltrimonium chloride are first mixed, then optionally trimethylolpropane tricaprylate and optionally an organic acid are mixed, and then the remaining components are mixed.

Preferably, the mixing comprises: sodium laureth sulfate, sodium lauroamphoacetate, optionally a polyquaternium salt and optionally guar hydroxypropyltrimonium chloride are first mixed, then optionally trimethylolpropane tricaprylate and optionally an organic acid, then water and optionally an ethylenediaminetetraacetic acid derivative, and finally the remaining components.

Preferably, the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, optional polyquaternary ammonium salt and optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with optional trimethylolpropane tricaprylate and optional organic acid, mixing with water and optional ethylene diamine tetraacetic acid derivatives, mixing with optional thickening agent, optional preservative and optional essence, and finally mixing with timosaponin enzymatic conversion product and/or timosaponin AIII.

According to the preferred embodiment, the components are mixed step by step according to the properties of the components, so that the mixing time can be effectively shortened, the mixing efficiency is improved, and the adverse effect on the performance of the components is avoided.

In a preferred embodiment, the mixing temperature of sodium laureth sulfate, sodium lauroamphoacetate, optionally a polyquaternium salt and optionally guar hydroxypropyltrimonium chloride is 60 to 70 ℃ and/or the mixing time is 10 to 20 min. The mixing temperature is typically, but not limited to, 60 deg.C, 61 deg.C, 62 deg.C, 63 deg.C, 64 deg.C, 65 deg.C, 66 deg.C, 67 deg.C, 68 deg.C, 69 deg.C or 70 deg.C; the mixing time is typically, but not limited to, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20 min.

Preferably, the mixing temperature when mixing with the optional trimethylolpropane tricaprylate and the optional organic acid is 75-85 ℃ and/or the mixing time is 15-30 min. The mixing temperature is typically, but not limited to, 75 deg.C, 76 deg.C, 77 deg.C, 78 deg.C, 79 deg.C, 80 deg.C, 81 deg.C, 82 deg.C, 83 deg.C, 84 deg.C or 85 deg.C; the mixing time is typically, but not limited to, 15min, 16min, 17min, 18min, 19min, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min or 30 min.

Preferably, the mixing temperature when mixing with water and optionally the ethylenediaminetetraacetic acid derivative is 75-85 ℃ and/or the mixing time is 5-10 min. The mixing temperature is typically, but not limited to, 75 deg.C, 76 deg.C, 77 deg.C, 78 deg.C, 79 deg.C, 80 deg.C, 81 deg.C, 82 deg.C, 83 deg.C, 84 deg.C or 85 deg.C; the above mixing time is typically, but not limited to, 5min, 6min, 7min, 8min, 9min or 10 min.

Preferably, the mixing temperature when mixing with the optional thickener, optional preservative and optional perfume is 35-45 ℃. The mixing temperature is typically, but not limited to, 35 deg.C, 36 deg.C, 37 deg.C, 38 deg.C, 39 deg.C, 40 deg.C, 41 deg.C, 42 deg.C, 43 deg.C, 44 deg.C or 45 deg.C.

Preferably, the mixing temperature when mixing with the timosaponin enzymatic hydrolysate and/or timosaponin AIII is 35-45 deg.C. The mixing temperature is typically, but not limited to, 35 deg.C, 36 deg.C, 37 deg.C, 38 deg.C, 39 deg.C, 40 deg.C, 41 deg.C, 42 deg.C, 43 deg.C, 44 deg.C or 45 deg.C.

When the mixing temperature and/or the mixing time are within the above ranges, the above components can be rapidly and uniformly mixed, the mixing uniformity is poor when the temperature is too low or the time is too short, and the energy cost and the time cost are increased when the temperature is too high or the time is too long.

Preferably, the mixing means comprises stirring.

Preferably, the stirring speed is 800-. The above stirring speed is typically, but not limited to, 800, 850, 900, 950 or 1000 rpm. When the stirring speed is in the above range, the components can be quickly and uniformly mixed, if the stirring speed is too slow, the mixing time can be too long, and if the stirring speed is too fast, the temperature of the mixed liquid during stirring is too fast, so that the mixed liquid is not easy to control and is not beneficial to mixing.

In a preferred embodiment, before the timosaponin enzymatic hydrolysate is mixed with the rest of the components, the method further comprises the step of preparing a timosaponin enzymatic hydrolysate into a timosaponin enzymatic hydrolysate suspension, and then mixing the timosaponin enzymatic hydrolysate with the rest of the components.

Preferably, the method further comprises the step of preparing timosaponin AIII into timosaponin AIII suspension or timosaponin AIII nanoliposome before mixing timosaponin AIII with the rest of the components, and then mixing with the rest of the components.

The timosaponin enzymolysis conversion product or timosaponin AIII is prepared into suspension, and then mixed with the rest components, so that the timosaponin enzymolysis conversion product or timosaponin AIII can realize good dispersibility before mixing, and is beneficial to the subsequent mixing process. The timosaponin AIII is prepared into nano liposome, which can be close to human cell membrane structure, and has certain moisture keeping effect on skin or hair.

The timosaponin enzymatic hydrolysate suspension is prepared by adding rhizoma anemarrhenae enzymatic hydrolysate into equal weight of distilled water, and performing ultrasonic treatment for 10min to disperse uniformly to obtain rhizoma anemarrhenae enzymatic hydrolysate suspension.

The timosaponin AIII suspension is prepared by adding timosaponin AIII into distilled water of equal weight, and performing ultrasonic treatment for 10min to disperse uniformly to obtain timosaponin enzymolysis product suspension.

The timosaponin AIII nano liposome is prepared by mixing timosaponin AIII solution with membrane material solution, and removing solvent and water to obtain lipid film; the membrane material comprises: a phospholipid, distearoylphosphatidylethanolamine-polyethylene glycol, or distearoylphosphatidylacetamide-methoxypolyethylene glycol; adding phosphate buffer solution, and hydrating to obtain timosaponin AIII liposome crude suspension; and performing ultrasonic treatment or high-pressure homogenization treatment at 40-60 ℃ to obtain the timosaponin AIII nano-liposome.

In a preferred embodiment, the timosaponin enzymatic hydrolysate suspension is prepared by the following method: and carrying out ultrasonic dispersion on the timosaponin enzymatic hydrolysate to obtain timosaponin enzymatic hydrolysate suspension.

Preferably, the timosaponin AIII suspension is prepared by the following method: and carrying out ultrasonic dispersion on the timosaponin AIII to obtain timosaponin AIII suspension.

Ultrasonic dispersion refers to a treatment process in which a dispersed phase (or dispersoid) is uniformly dispersed in a solvent (or dispersion medium, continuous phase) by using ultrasonic waves. The ultrasonic dispersion has high dispersion efficiency and good dispersion effect, and does not have adverse effect on the structure and properties of the dispersed phase.

Preferably, the ultrasonic dispersion time is 8-12 min. The ultrasonic dispersion time is typically, but not limited to, 8min, 8.5min, 9min, 9.5min, 10min, 10.5min, 11min, 11.5min or 12 min.

Preferably, the solvent used for ultrasonic dispersion comprises water.

Preferably, the weight ratio of the timosaponin enzymolysis conversion product or timosaponin AIII to the solvent used for ultrasonic dispersion is 1: (0.5-1.5). The above weight ratio is typically, but not limited to, 1: 0.5, 1: 0.7, 1: 1. 1: 1.2 or 1: 1.5. when the weight ratio is within the above range, the dispersion efficiency of the timosaponin enzymatic hydrolysate or timosaponin AIII is higher, and if the weight ratio is too high or too low, the dispersion speed is reduced and the dispersion efficiency is reduced.

In a preferred embodiment, the timosaponin AIII nanoliposome is prepared by the following method: mixing the timosaponin AIII solution with the membrane material solution, and removing the solvent and water to obtain a lipid membrane; and then sequentially hydrating and homogenizing the lipid film to obtain the timosaponin AIII nano-liposome. The water solubility of timosaponin AIII can be effectively improved by preparing liposome, and the liposome has the advantages of easily available raw materials, high encapsulation efficiency, good stability, particle size range of 25-80nm, and easy absorption.

"timosaponin AIII solution" refers to methanol, ethanol, chloroform or acetone solution of timosaponin AIII; the membrane material solution is methanol, ethanol, chloroform or acetone solution of the membrane material. The step of hydration is that timosaponin AIII solution is mixed with membrane material solution, then solvent and water are removed to obtain a lipid film, and then the lipid film is hydrated in phosphate buffer solution, wherein the concentration of the phosphate buffer solution is 0.05-0.1 mol/L, and the pH value is 7.2-7.6; the hydration conditions are as follows: treating at 45-50 deg.c for 30-120 min.

The homogenization refers to dispersing the timosaponin AIII hydration liquid in a high-pressure homogenizer, and circulating for 2-6 times under the condition of 10000-30000 PSI.

Preferably, the means of homogenization comprises high pressure homogenization. Preferably, the high pressure homogenization conditions include: circulating for 2-6 times under the condition of 10000-30000 PSI. For example, cycling 3 times under 20000PSI conditions, 6 times under 10000PSI conditions, or 2 times under 30000PSI conditions, etc.

Preferably, the membrane material comprises at least one of phospholipid, distearoylphosphatidylethanolamine-polyethylene glycol or distearoylphosphatidylacetamide-methoxypolyethylene glycol. Such membrane materials include, but are not limited to, phospholipids, distearoylphosphatidylethanolamine-polyethylene glycol, distearoylphosphatidylacetamide-methoxypolyethylene glycol, a combination of phospholipids and distearoylphosphatidylethanolamine-polyethylene glycol, a combination of distearoylphosphatidylethanolamine-polyethylene glycol and distearoylphosphatidylacetamide-methoxypolyethylene glycol, a combination of phospholipids and distearoylphosphatidylacetamide-methoxypolyethylene glycol, or a combination of phospholipids, distearoylphosphatidylethanolamine-polyethylene glycol, and distearoylphosphatidylacetamide-methoxypolyethylene glycol. The addition of distearoyl phosphatidyl ethanolamine-polyethylene glycol or distearoyl phosphatidyl acetamide-methoxy polyethylene glycol can prolong the circulation time of the liposome in body blood, and the drug effect is longer.

It should be noted that, the specific process for removing the solvent and the moisture is selected from those commonly used in the art or related fields, and the present invention is not limited to this, for example, a rotary vacuum dryer may be selected to dry the solvent and the moisture, and then the solvent and the moisture are removed.

The present invention will be described in further detail with reference to examples and comparative examples.

Example 1

A shampoo comprises the following components in percentage by weight: 8% of sodium laureth sulfate, 10% of cocamidopropyl betaine, 0.5% of sodium lauroamphoacetate, 5% of timosaponin enzymatic hydrolysis conversion product and the balance of water.

Example 2

A shampoo comprises the following components in percentage by weight: 8% of sodium laureth sulfate, 20% of sodium laureth sulfate, 18% of sodium stearate, 5% of cocoyl stearate, 7% of sodium chloride, 4% of ethylene glycol stearate, 1% of saponin, 4% of glycerol, 5% of timosaponin enzymatic hydrolysis converted product and the balance of water.

Example 3

A shampoo comprises the following components in percentage by weight: 9% of sodium laureth sulfate, 4% of cocamidopropyl betaine, 1% of sodium lauroamphoacetate, 5% of timosaponin enzymatic hydrolysis converted product and the balance of water.

Example 4

A shampoo comprises the following components in percentage by weight: 13% of sodium laureth sulfate, 9% of cocamidopropyl betaine, 5% of sodium lauroamphoacetate, 5% of timosaponin enzymatic hydrolysis converted substance and the balance of water.

Unlike examples 1-2, the contents of the components in examples 3-4 are within the preferred range of the present invention.

Example 5

A shampoo comprises the following components in percentage by weight: 9.5 percent of sodium laureth sulfate, 5 percent of cocamidopropyl betaine, 2 percent of sodium lauroyl amphoacetate, 5 percent of timosaponin enzymatic hydrolysis converted substance and the balance of water.

Example 6

A shampoo comprises the following components in percentage by weight: 11% of sodium laureth sulfate, 8% of cocamidopropyl betaine, 4% of sodium lauroamphoacetate, 5% of timosaponin enzymatic hydrolysis converted product and the balance of water.

Unlike examples 3-4, the contents of each component in examples 5-6 are within the further preferred range of the present invention.

Example 7

A shampoo comprises the following components in percentage by weight: 11% of sodium laureth sulfate, 8% of cocamidopropyl betaine, 4% of sodium lauroamphoacetate, 0.5% of timosaponin AIII and the balance of water.

Different from example 6, in this embodiment, the timosaponin a iii enzymatic hydrolysate is replaced by timosaponin a iii, and the content of timosaponin a iii is different from that of the timosaponin enzymatic hydrolysate in example 6.

Example 8

A shampoo comprises the following components in percentage by weight: 11% of sodium laureth sulfate, 8% of cocamidopropyl betaine, 4% of sodium lauroamphoacetate, 2% of timosaponin enzymatic hydrolysis converted product, 1% of timosaponin AIII and the balance of water.

Different from example 6, in this example, timosaponin enzymatic hydrolysate 4% was replaced by timosaponin enzymatic hydrolysate 2% and timosaponin aiii 1%.

Examples 9 to 12

A shampoo is different from the shampoo in the embodiment 8, in the embodiment 9-12, polyquaternium-10 is also included, and the weight percentage of the polyquaternium-10 is respectively 3 percent, 0.5 percent, 1 percent and 2.5 percent.

The weight percent of polyquaternium-10 in examples 10-12 is within the preferred range of the present invention.

Examples 13 to 16

A shampoo, different from the shampoo of the embodiment 12, comprises guar gum hydroxypropyl trimethyl ammonium chloride in the embodiments 13 to 16, wherein the weight percentage of the guar gum hydroxypropyl trimethyl ammonium chloride is respectively 0.05 percent, 0.1 percent, 0.9 percent and 0.5 percent.

The weight percent guar hydroxypropyltrimonium chloride in examples 14-16 is within the preferred range of the invention.

Examples 17 to 20

A shampoo is different from the shampoo in the embodiment 16 in that the shampoo in the embodiments 17 to 20 further comprises citric acid, and the weight percentage of the citric acid is respectively 1 percent, 0.2 percent, 0.4 percent and 0.7 percent.

The weight percent citric acid content of examples 18-20 is within the preferred range of the present invention.

Examples 21 to 24

A shampoo is different from the shampoo in the embodiment 20, in the embodiment 21-24, disodium ethylene diamine tetraacetate is further included, and the weight percentage of the disodium ethylene diamine tetraacetate is respectively 1%, 0.1%, 0.2% and 0.5%.

The weight percent of disodium edetate in examples 20-24 is within the preferred range of the present invention.

Examples 25 to 26

A shampoo, which is different from the shampoo prepared in the embodiment 24, in the embodiments 25 to 27, a thickening agent, a preservative and an essence are further included, wherein the thickening agent is 0.1%, 0.2% and 0.4% by weight respectively, the preservative is 0.1%, 0.2% and 0.3% by weight respectively, and the essence is 0.5%, 2% and 5% by weight respectively.

The preparation method of the shampoo in the above embodiments comprises the following steps: mixing the above components at 40 deg.C to obtain the shampoo.

Example 28

A method of making the shampoo of embodiment 27, comprising: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, polyquaternium-10 and guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with trimethylolpropane tricaprylate and citric acid, then mixing with water and disodium ethylene diamine tetraacetate, then mixing with a thickening agent, a preservative and essence, and finally mixing with a timosaponin enzymolysis conversion product and timosaponin AIII to obtain the shampoo;

wherein the mixing temperature of the sodium laureth sulfate, the sodium lauroamphoacetate, the polyquaternium-10 and the guar gum hydroxypropyl trimethyl ammonium chloride is 55 ℃, and the mixing time is 8 min;

mixing with trimethylolpropane tricaprylate and citric acid at 88 deg.C for 10 min;

mixing with water and disodium ethylene diamine tetraacetate at 70 deg.C for 15 min;

mixing with thickener, antiseptic and essence at 50 deg.C;

mixing with timosaponin enzymolysis product and timosaponin AIII at 50 deg.C;

the mixing was carried out by stirring at 1200 rpm.

Example 29

The shampoo of example 27 is prepared by mixing sodium laureth sulfate, sodium lauroamphoacetate, polyquaternium-10 and guar hydroxypropyltrimonium chloride at 65 ℃ for 15min, which is different from example 28.

Example 30

A shampoo of example 27 was prepared in a manner different from that of example 29, except that in this example, the mixing temperature was 80 ℃ and the mixing time was 20min when mixing the shampoo with trimethylolpropane tricaprylate and citric acid.

Example 31

The shampoo of example 27 was prepared by a method different from example 30, in this example, the mixing temperature of water and disodium edetate was 80 ℃ and the mixing time was 8 min.

Example 32

The shampoo of example 27 was prepared in a manner different from that of example 31, and in this example, the mixing temperature was 40 ℃ when the shampoo was mixed with the thickener, the preservative and the essence.

Example 33

The shampoo of example 27 is prepared, in contrast to example 32, by mixing timosaponin A III with the enzymatic converted product of timosaponin at a mixing temperature of 40 ℃.

Example 34

The shampoo preparation process described in example 27 was conducted at a stirring speed of 900rpm, unlike example 33.

Example 35

The method of preparing a shampoo in embodiment 27, which is different from embodiment 34, in this embodiment, before the timosaponin enzymatic hydrolysate is mixed with the remaining components, the method further includes a step of preparing a timosaponin enzymatic hydrolysate into a timosaponin enzymatic hydrolysate suspension, and then mixing the timosaponin enzymatic hydrolysate suspension with the remaining components;

the timosaponin enzymolysis conversion product suspension is prepared by the following method: carrying out enzymolysis on the timosaponin converted substance and water according to the ratio of 1: 1, and ultrasonically dispersing for 10min to obtain timosaponin enzymatic hydrolysis conversion substance suspension.

Example 36

A method for producing a shampoo of embodiment 27, which is different from embodiment 35 in that, in this embodiment, the method further includes the step of preparing timosaponin aiii into timosaponin aiii nanoliposomes before mixing timosaponin aiii with the remaining components, and then mixing the timosaponin aiii nanoliposomes with the remaining components;

the timosaponin AIII nano liposome is prepared by the following method: weighing 2.5mg timosaponin AIII, dissolving in 1.25mL methanol, weighing 23.5mg egg yolk lecithin and 9.4mg distearoylphosphatidylethanolamine-polyethylene glycol 2000(DSPE-PEG2000), dissolving in 2mL chloroform solution, ultrasonic dissolving, mixing the above solutions in a round bottom flask, blowing with nitrogen gas to remove methanol and chloroform, and allowing a uniform lipid film to form on the wall of the round bottom flask. Drying under reduced pressure at 45 deg.C under-0.09 MPa to remove residual solvent and water, adding 0.6mL of 0.01mol/L phosphate buffer (pH 7.4), and hydrating in water bath at 45 deg.C for 1 hr to obtain timosaponin AIII liposome crude suspension. And (3) carrying out ultrasonic treatment on the crude suspension of the timosaponin AIII liposome for 3 times at the ultrasonic frequency of 50Hz and the power of 200W, wherein the ultrasonic treatment time is 3min each time, so as to obtain the timosaponin AIII nano liposome.

Example 37

A hair conditioner containing timosaponin enzymatic hydrolysate and/or timosaponin AIII comprises the following components in parts by weight: 5% of octadecanol, 3% of stearamidopropyl dimethyl tertiary amine, 4% of propylene glycol, 4% of dimethyl silicone oil, 450.3% of polyoxyethylene ether, 1.4% of citric acid, 0.4% of a mixture of dimethyloldimethylhydantoin and 3-iodo-2 propynyl butyl carbamate, 0.3% of essence, 0.3% of disodium ethylenediamine tetraacetate, 5% of timosaponin AIII and 76.3% of deionized water.

Example 38

A shower gel containing timosaponin enzymatic hydrolysate and/or timosaponin AIII comprises the following components in parts by weight: 15% of sodium laureth sulfate, 5% of ammonium laureth sulfate, 3% of cocamidopropyl betaine, 3% of cocamide DEA, 4% of humectant, 0.2% of sodium chloride, 0.1% of essence, 0.02% of DMDM hydantoin, 0.3% of milk, 0.3% of pH regulator, 5% of timosaponin enzymatic hydrolysis conversion product and 68.8% of deionized water.

Example 39

A hand sanitizer containing timosaponin enzymatic hydrolysate and/or timosaponin AIII comprises the following components in parts by weight: 9% of sodium cocoyl amphopropionate, 6% of dodecyl dimethyl amine oxide, 1% of lauryl oleate, 3% of glycerol, 5% of timosaponin enzymatic hydrolysis converted substance and 76% of deionized water.

Comparative example 1

A shampoo comprises the following components in percentage by weight: 15% of sodium laureth sulfate, 3% of cocamidopropyl betaine, 6% of sodium lauroamphoacetate, 0.4% of timosaponin enzymatic hydrolysis converted product and the balance of water.

Comparative example 2

A shampoo comprises the following components in percentage by weight: sodium laureth sulfate 8%, cocamidopropyl betaine 10%, sodium lauroamphoacetate 0.5%, timosaponin AIII 0.4%, and water in balance.

The content of the timosaponin enzymatic conversion product in comparative examples 1-2 is out of the range provided by the present invention.

Comparative example 3

A shampoo comprises the following components in percentage by weight: 9% of sodium laureth sulfate, 4% of cocamidopropyl betaine, 1% of sodium lauroamphoacetate and the balance of water.

Unlike example 1, the present comparative example did not contain the timosaponin enzymatic hydrolysate.

Comparative example 4

A shampoo comprises the following components in percentage by weight: 9 percent of sodium laureth sulfate, 4 percent of cocamidopropyl betaine, 1 percent of sodium lauroamphoacetate, 0.5 percent of methyl salicylate and the balance of water.

Unlike example 1, in this comparative example, the timosaponin enzymatic conversion product was replaced with methyl salicylate.

Comparative example 5

Haifeisu anti-dandruff shampoo (refreshing oil removing type).

Comparative example 6

Anti-dandruff shampoo (refreshing oil-control type) for clearing men.

The timosaponin enzymatic hydrolysate related in each embodiment and each proportion is prepared by the following method:

(1) preparing an ethanol extract of rhizoma anemarrhenae: 60g of rhizoma anemarrhenae (decoction pieces) is weighed, 6 times of 50% ethanol is added, heating reflux is carried out, the boiling state is kept, the extraction time is 2 hours each time, and the extraction is carried out for 2 times. Filtering, mixing extractive solutions, rotary evaporating under reduced pressure, and recovering ethanol to obtain timosaponin ethanol extract with final volume of 1.5 g/mL.

(2) Preparing an enzymolysis conversion product of timosaponin:

weighing 4g of anemarrhena ethanol extract (equivalent to 6g of anemarrhena medicinal material) and 4g of beta-glucosidase (50U/mg), placing in a conical flask with a plug, adding 200mL of acetic acid-sodium acetate buffer solution with the pH value of 4.0, and placing in an air bath constant temperature oscillator for shaking for 2 h. Drying in vacuum drying oven at 60 deg.C under reduced pressure to obtain timosaponin enzymolysis conversion product I.

(3) Further purifying enzymolysis conversion product of rhizoma anemarrhenae extract

The method comprises the following steps: ammonia water washing and purification: taking out after enzymolysis, mixing, centrifuging at 3000r/min for 10min, and discarding supernatant. Adding 200ml ammonia solution into the precipitate, stirring for 10min, mixing, centrifuging at 3000r/min for 10min, removing supernatant, and collecting precipitate. Drying and collecting to obtain the timosaponin enzymatic hydrolysate II-1.

The second method comprises the following steps: washing and purifying with NaOH solution: after the enzymolysis is finished, taking 200ml of the enzymolysis liquid, adding 80ml of 1% NaOH solution (taking 1g of NaOH solid, adding distilled water to 100ml, and obtaining the product), mixing uniformly, centrifuging at the rotating speed of 3000r/min for 10min, removing supernatant, and taking precipitate. Drying and collecting to obtain the timosaponin enzymatic hydrolysate II-2.

(4) And (3) determining the content of timosaponin AIII of the enzymatic hydrolysate:

chromatographic conditions are as follows: the chromatographic column is a Platisil C18 chromatographic column (4.6 mm. times.250 mm, 5 μm); mobile phase: the methanol-water ratio is 85: 15; flow rate: 1 mL/min; the sample injection amount is 20 mu L; column temperature: 30 ℃; the temperature of the evaporative light scattering detector was 60 ℃ and the flow rate of the atomizing gas was 1.5L/min.

Weighing 10.00mg of timosaponin AIII reference substance, precisely weighing, placing in a 10mL volumetric flask, dissolving with methanol, metering to scale mark, and mixing to obtain timosaponin AIII reference substance stock solution with concentration of 1.00 mg/mL. Preparing control solutions with timosaponin AIII concentration of 49.35, 98.70, 246.8, 493.5, 789.6, and 987.0 μ g/mL, and respectively injecting into high performance liquid chromatograph. And (3) drawing a standard curve by taking the common logarithm of the concentration of the timosaponin AIII reference substance as a horizontal coordinate (X) and taking the logarithm value of each corresponding peak area as a vertical coordinate (Y), and calculating a regression equation. Precisely weighing 10mg of the zymolysis conversion product, placing in a 25mL volumetric flask, fixing the volume with methanol, ultrasonically dissolving, filtering with a 0.45 mu m microporous membrane, and injecting into a liquid chromatograph for content determination.

The results show that the contents of timosaponin AIII in the zymolytic conversion products I, II-1 and II-2 are 52.47% + -0.32% (RSD is 0.5%), 62.13% + -0.86% and 61.36% + -0.45%, respectively. Therefore, timosaponin enzymatic hydrolysate II-2 was selected as a raw material in each example and comparative example.

Inhibition of the Ring test

The shampoos in examples 6 to 7 and comparative examples 1 to 6 were subjected to the bacteriostatic ring test:

preparation of test pieces: taking Xinhua I qualitative filter paper, beating the Xinhua I qualitative filter paper into a circular filter paper sheet with the diameter of 5mm by a puncher, sterilizing by pressure steam, taking a plurality of sample pieces dried after sterilization treatment, respectively dipping a little of shampoo in examples 6-7 and comparative examples 1-6 on the sample pieces by sterile tweezers, and smearing the sample pieces uniformly as much as possible.

Preparation of the plate: activated malassezia furfur and malassezia globosa are prepared into bacterial suspension of 106 cfu/mL-107 cfu/mL, and 0.3mL of the bacterial suspension is smeared on a 12cm Leeming & Notman culture medium plate. After the plate containing the bacteria was left to stand for 10min, the plate cover was opened in a sterile hood, and the plate was dried by blowing with sterile air (about 20 min).

Determination of the bacteriostatic effect: to each plate were attached 4 test coupons, 1 negative control (no test shampoo) coupon, and a total of 5. After the sample is placed, the sample is lightly pressed by using sterile tweezers to make the sample tightly attached to the surface of the flat plate. The plate is covered, placed in a constant temperature incubator at 32 ℃ for inverted culture for 7 days, and the diameter of the inhibition zone is measured and recorded by a vernier caliper.

Referring to table 2, the results show that the diameters of inhibition zones of the timosaponin enzymatic hydrolysate shampoo (example 6) on malassezia furfur and malassezia globosa isolated from human bodies are 25mm and 22mm respectively, and the diameters of inhibition zones of the timosaponin AIII shampoo (example 7) on malassezia furfur and malassezia globosa isolated from human bodies are 22mm and 21mm respectively, and the effects are superior to those of common sea-flying-silk anti-dandruff shampoo (comparative example 5) and clear-up anti-dandruff shampoo (comparative example 6) in the market. Meanwhile, the shampoo does not contain the timosaponin converted product shampoo (comparative examples 3-4) and the low-concentration timosaponin zymose converted product shampoo and the timosaponin AIII shampoo (comparative examples 1-2) have weak bacteriostatic action on malassezia furfur and malassezia globosa separated from a human body, and the timosaponin zymohydrolysis converted product and the timosaponin AIII play main bacteriostatic action in the shampoo. The same bacteriostatic ring test is carried out on other examples, and the results show that the other examples also have good inhibitory effect on malassezia furfur and malassezia globosa, and the bacteriostatic effect is superior to each proportion.

TABLE 2 bacteriostatic ring test results (bacteriostatic circle diameter, mm)

Test of Using Effect

Volunteers were divided equally into two groups-control and test groups, 60 groups, 120 in total, according to dandruff severity. The control group used the shampoo of comparative example 3, and the test group used the shampoo of example 3, and the test group was carried out by the same investigator under natural and sufficient light, and the light in the room should be kept consistent every follow-up visit. Photographs were observed before, 2 weeks after, 4 weeks after the test. The evaluation indexes mainly comprise: dandruff severity score, scalp itch score (0 for no symptoms, 1-4 for mild to severe severity), and the data (tables 3 and 4) are from the interview questionnaire with human subjects.

Improvement of scalp itching: the experimental results show that after the shampoo is used for 4 weeks, compared with the control group and the test group before and after the shampoo is used, the scalp itch of the test group is obviously improved (P is less than 0.05, see table 5), and the improvement condition of the control group has no statistical significance (P is more than 0.05, see table 5).

Dandruff improvement: the experimental results show that after the shampoo is used for 4 weeks, compared with the shampoo before the shampoo is used, the dandruff of the experimental group is obviously reduced (P is less than 0.05, see table 5), the improvement condition of the control group is not statistically significant (P is more than 0.05), and the dandruff of the experimental group is obviously reduced better than that of the control group compared with the experimental group and the control group.

No adverse reactions such as irritation and the like appear in volunteers during the experiment. The results show that the timosaponin enzymatic hydrolysate can be added into shampoo to effectively inhibit dandruff breeding and improve pruritus.

TABLE 3 scalp itching of volunteers before and after shampoo application

TABLE 4 dandruff condition of volunteers before and after shampoo use

TABLE 5 statistical differences in test results (P-value) between test and control groups

While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims (10)

1. A cosmetic is characterized by comprising an timosaponin enzymatic hydrolysate and/or timosaponin AIII, wherein the weight percentage content of the timosaponin enzymatic hydrolysate and/or timosaponin AIII is 0.5% -5%;

preferably, the cosmetic comprises a shampoo, a conditioner or a hand sanitizer.

2. The cosmetic according to claim 1, wherein the weight percentage of timosaponin enzymatic hydrolysate and/or timosaponin AIII is 1-5%;

preferably, the shampoo further comprises at least one of sodium laureth sulfate, cocamidopropyl betaine, or sodium lauroamphoacetate;

preferably, the sodium laureth sulfate is present in an amount of 9% to 13%, preferably 9.5% to 11%, by weight;

preferably, the weight percentage content of cocamidopropyl betaine is 4% to 9%, preferably 5% to 8%;

preferably, the weight percentage content of the sodium lauroamphoacetate is 1 to 5 percent, and preferably 2 to 4 percent;

preferably, the shampoo comprises the following components in percentage by weight: 9-13% of sodium laureth sulfate, 4-9% of cocamidopropyl betaine, 1-5% of sodium lauroamphoacetate, 0.5-5% of timosaponin enzymolysis conversion product and/or timosaponin AIII and the balance of water; preferably, the shampoo comprises the following components in percentage by weight: 9.5-11% of sodium laureth sulfate, 5-8% of cocamidopropyl betaine, 2-4% of sodium lauroamphoacetate, 1-5% of timosaponin enzymolysis conversion product and/or timosaponin AIII and the balance of water.

3. The cosmetic of claim 2, wherein said shampoo further comprises at least one of a softener, a moisturizer, or a chelating agent;

preferably, the shampoo further comprises at least one of a thickener, a preservative or a fragrance.

4. The cosmetic according to claim 3, characterized in that the softener comprises polyquaternium and/or guar hydroxypropyltrimonium chloride;

preferably, the polyquaternium comprises polyquaternium-7 and/or polyquaternium-10;

preferably, the weight percentage content of the polyquaternium is 0.5 to 2.5 percent;

preferably, the weight percentage content of the guar gum hydroxypropyl trimethyl ammonium chloride is 0.1-0.9%;

preferably, the humectant comprises trimethylolpropane tricaprylate;

preferably, the weight percentage content of the trimethylolpropane tricaprylate is 0.1-0.6%;

preferably, the chelating agent comprises an organic acid and/or an ethylenediaminetetraacetic acid derivative;

preferably, the organic acid comprises citric acid and/or tartaric acid;

preferably, the weight percentage content of the organic acid is 0.2 to 0.7 percent;

preferably, the ethylenediaminetetraacetic acid derivatives include ethylenediaminetetraacetic acid sodium salt;

preferably, the sodium salt of ethylenediaminetetraacetic acid comprises disodium ethylenediaminetetraacetate and/or tetrasodium ethylenediaminetetraacetate;

preferably, the weight percentage content of the ethylene diamine tetraacetic acid derivative is 0.1% -0.5%;

preferably, the weight percentage content of the thickening agent is 0.1% -0.4%;

preferably, the preservative is present in an amount of 0.1% to 0.3% by weight;

preferably, the essence accounts for 0.5 to 5 weight percent.

5. A method for producing a cosmetic according to any one of claims 1 to 4, comprising: mixing the above components uniformly to obtain the cosmetic.

6. The method for preparing a cosmetic according to claim 5, wherein the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, optional polyquaternary ammonium salt and optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with optional trimethylolpropane tricaprylate and optional organic acid, and then mixing with the rest components;

preferably, the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, an optional polyquaternary ammonium salt and an optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with an optional trimethylolpropane tricaprylate and an optional organic acid, mixing with water and an optional ethylene diamine tetraacetic acid derivative, and finally mixing with the rest components;

preferably, the mixing comprises: firstly, mixing sodium laureth sulfate, sodium lauroamphoacetate, optional polyquaternary ammonium salt and optional guar gum hydroxypropyl trimethyl ammonium chloride, then mixing with optional trimethylolpropane tricaprylate and optional organic acid, mixing with water and optional ethylene diamine tetraacetic acid derivatives, mixing with optional thickening agent, optional preservative and optional essence, and finally mixing with timosaponin enzymatic conversion product and/or timosaponin AIII.

7. The method for preparing a cosmetic according to claim 6, wherein the mixing temperature of sodium laureth sulfate, sodium lauroamphoacetate, optionally a polyquaternium salt, and optionally guar hydroxypropyltrimonium chloride is 60 to 70 ℃, and/or the mixing time is 10 to 20 min;

preferably, the mixing temperature when mixing with the optional trimethylolpropane tricaprylate and the optional organic acid is 75-85 ℃, and/or the mixing time is 15-30 min;

preferably, the mixing temperature when mixing with water and optionally the ethylenediaminetetraacetic acid derivative is 75-85 ℃ and/or the mixing time is 5-10 min;

preferably, the mixing temperature when mixing with the optional thickener, optional preservative and optional perfume is 35-45 ℃;

preferably, the mixing temperature when the timosaponin enzymatic hydrolysate and/or timosaponin AIII are mixed is 35-45 ℃;

preferably, the mixing means comprises stirring;

preferably; the stirring speed was 800-1000 rpm.

8. The method for preparing a cosmetic according to any one of claims 5 to 7, wherein before the enzymatic hydrolysis transformant of timosaponin is mixed with the remaining ingredients, the method further comprises a step of preparing the enzymatic hydrolysis transformant of timosaponin into a timosaponin enzymatic hydrolysis transformant suspension, and then mixing with the remaining ingredients;

preferably, the method further comprises the step of preparing timosaponin AIII into timosaponin AIII suspension or timosaponin AIII nanoliposome before mixing timosaponin AIII with the rest of the components, and then mixing with the rest of the components.

9. The method for preparing a cosmetic according to claim 8, wherein the timosaponin enzymatic hydrolysate suspension is prepared by: ultrasonically dispersing the timosaponin enzymatic hydrolysate to obtain timosaponin enzymatic hydrolysate suspension;

preferably, the timosaponin AIII suspension is prepared by the following method: ultrasonically dispersing timosaponin AIII to obtain timosaponin AIII suspension;

preferably, the ultrasonic dispersion time is 8-12 min;

preferably, the solvent used for ultrasonic dispersion comprises water;

preferably, the weight ratio of the timosaponin enzymolysis conversion product or timosaponin AIII to the solvent used for ultrasonic dispersion is 1: (0.5-1.5).

10. The method for preparing a cosmetic according to claim 8, wherein the timosaponin AIII nanoliposome is prepared by the following method: mixing the timosaponin AIII solution with the membrane material solution, and removing the solvent and water to obtain a lipid membrane; then sequentially hydrating and homogenizing the lipid film to obtain timosaponin AIII nano-liposome;

preferably, the means of homogenization comprises high pressure homogenization;

preferably, the high-pressure homogenizing condition comprises circulation for 2-6 times under 10000-30000 PSI conditions;

preferably, the membrane material comprises at least one of phospholipid, distearoylphosphatidylethanolamine-polyethylene glycol or distearoylphosphatidylacetamide-methoxypolyethylene glycol.