CN113122602A

CN113122602A - Preparation method and application of quaternized hydrolyzed wheat protein in special anti-hair loss shampoo for women

Info

Publication number: CN113122602A
Application number: CN202110412072.7A
Authority: CN
Inventors: 王峰; 王奕尧
Original assignee: Xi'an Blue Wind Biotechnology Co ltd
Current assignee: Xi'an Blue Wind Biotechnology Co ltd
Priority date: 2018-02-08
Filing date: 2018-02-08
Publication date: 2021-07-16
Also published as: CN108042438A

Abstract

The invention discloses a preparation method and application of quaternized hydrolyzed wheat protein in special anti-hair loss shampoo for women, wherein the quaternized hydrolyzed wheat protein has opsonization of natural substances such as protein and the like and adsorbability of quaternary ammonium salt. By introducing quaternary ammonium ions into the tail end of the hydrolyzed wheat protein, the isoelectric point of the protein is improved, and the adsorbability of the protein to hair is increased, so that the adhesiveness of the quaternized wheat hydrolyzed protein is superior to that of the hydrolyzed wheat protein, the conditioning capability is stronger than that of the hydrolyzed protein, and the effects of improving static accumulation, smoothing hair and the like are more obvious.

Description

Preparation method and application of quaternized hydrolyzed wheat protein in special anti-hair loss shampoo for women

The application is a divisional application with application date of 2018, 02 and 08, application number of 201810125873.3, and invention name of hair loss preventing shampoo special for women and a preparation method thereof.

Technical Field

The invention belongs to the technical field of shampoo, and particularly relates to a preparation method and application of quaternized hydrolyzed wheat protein in special anti-hair loss shampoo for women.

Background

In modern beauty, hair is also one of aesthetic elements and is an important component for beauty, and a head of the hair is elegant, smooth, black and bright and can transmit youthful vitality information to bring beauty and beauty to people, while hair loss can seriously affect beauty.

The invention patent with application number 201510499409.7 discloses an anti-hair loss shampoo, which is prepared from the following components in parts by weight: 20-30 parts of rice powder, 10-20 parts of ginseng, 10-20 parts of capsicum annuum, 10-20 parts of cactus and 10-20 parts of asarum. The shampoo is prepared by rice powder, four traditional Chinese medicines and a common shampoo matrix, can accelerate brain blood circulation and provide enough nutrition, thereby increasing brain circulation, effectively resisting cerebral anoxia, promoting energy metabolism of brain cells and metabolic activity of neurotransmitter in brain, and ensuring that the shampoo directly acts on cerebral cortex. The shampoo can quickly remove oil stains and dandruff in hair, eliminate excessive oil secretion, discharge harmful substances damaging the hair, keep the hair black, glossy and smooth, and has the effects of removing the oil stains, removing the dandruff, stopping itching of the head, preventing alopecia and the like.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a preparation method and application of quaternized hydrolyzed wheat protein in special anti-hair loss shampoo for women.

The purpose of the invention is realized by the following technical scheme:

the special anti-hair loss shampoo for women comprises water, ammonium laureth sulfate, cocamidopropyl betaine, sodium lauroyl sarcosinate, cacumen Platycladi extract, radix Polygoni Multiflori extract, ethylene glycol distearate, rhodiola rosea extract, ginseng root extract, guar gum hydroxypropyl trimethyl ammonium chloride, sodium chloride, hydrolyzed wheat protein, essence, panthenol, ganoderma atrum extract, cetostearyl alcohol, citric acid, EDTA disodium, methylparaben and methylisothiazolinone.

Specifically, the special anti-hair loss shampoo for women is composed of the following raw materials in parts by weight: 6-10 wt% of ammonium laureth sulfate, 5-8 wt% of cocamidopropyl betaine, 2-3 wt% of sodium lauroyl sarcosinate, 0.9-1.5 wt% of cacumen biotae extract, 1.2-1.6 wt% of polygonum multiflorum root extract, 1.1-1.6 wt% of ethylene glycol distearate, 0.7-1.8 wt% of rhodiola rosea extract, 0.7-3.2 wt% of ginseng root extract, 0.5-1.5 wt% of guar hydroxypropyl trimethylammonium chloride, 0.4-0.8 wt% of sodium chloride, 0.5-2.0 wt% of hydrolyzed wheat protein, 0.5-1.2 wt% of essence, 0.1-0.3 wt% of panthenol, 0.3-0.5 wt% of ganoderma atrum extract, 0.2-0.5 wt% of cetearyl alcohol, 0.15-0.35 wt% of citric acid, 0.1-0.3 wt% of disodium EDTA, 0.1-0.2 wt% of methylparaben, 0.02-0.2 wt% of methyl isothiazolinone, and the balance of water.

In the invention, the preparation process of the cacumen biotae extract comprises the following steps: crushing the cacumen biotae, and sieving the cacumen biotae with a 60-80-mesh sieve to obtain cacumen biotae powder; mixing cacumen biotae powder and 70-80% by volume of ethanol water according to a material-liquid ratio of 1: (20-30) (g/mL) and uniformly mixing, and extracting at 70-80 ℃ for 3-4 hours to obtain a cacumen biotae extracting solution; adding a flocculant aqueous solution with the mass fraction of 2-3% into the cacumen biotae extracting solution, wherein the volume ratio of the cacumen biotae extracting solution to the flocculant aqueous solution is 1: (0.1-0.15), uniformly mixing, standing for 12-24 hours at 20-23 ℃, filtering by adopting 100-200 meshes of filter cloth, and collecting filtrate; and drying the filtrate for 6-10 hours at the temperature of 40-50 ℃ and the vacuum degree of 0.08-0.09 MPa to obtain the cacumen biotae extract. Wherein, the flocculating agent can be selected from one or a combination of gelatin and chitosan.

The preparation of the polygonum multiflorum root extract, the rhodiola rosea extract and the ganoderma atrum extract is carried out with reference to the preparation of the cacumen biotae extract, and the cacumen biotae is replaced by the polygonum multiflorum root, the rhodiola rosea and the ganoderma atrum respectively to obtain the polygonum multiflorum root extract, the rhodiola rosea extract and the ganoderma atrum extract.

In some embodiments of the invention, the preparation of the ginseng root extract is performed with reference to the preparation of the cacumen biotae extract, replacing cacumen biotae with ginseng root, resulting in a ginseng root extract.

In some embodiments of the present invention, the ginseng root extract is prepared by the following steps: crushing ginseng roots, and sieving the crushed ginseng roots with a 60-80-mesh sieve to obtain ginseng root powder; cleaning glutinous rice, adding water which is 5-10 times of the weight of the glutinous rice, soaking for 8-12 hours, taking out, draining, wrapping with gauze, putting into a steamer, steaming at 100 ℃ for 30-40 minutes, taking out, and putting into a fermentation device; adding ginseng root powder, water, distiller's yeast and yeast into a fermentation device, wherein the addition amounts of the ginseng root powder, the water, the distiller's yeast and the yeast are respectively 20-30%, 1-1.5%, 2-3% and 0.2-0.3% of the weight of the sticky rice, uniformly mixing, and fermenting for 15-20 days at 15-17 ℃; after fermentation is finished, filtering a fermentation product by using 80-100-mesh filter cloth, and collecting filtrate; and drying the filtrate for 10-16 hours at the temperature of 40-50 ℃ and the vacuum degree of 0.06-0.08 MPa to obtain the ginseng root extract.

The hydrolyzed wheat protein is one or a mixture of more of acid hydrolyzed wheat protein, quaternized hydrolyzed wheat protein and amidase hydrolyzed wheat protein.

The preparation process of the acid hydrolysis wheat protein comprises the following steps: preparing a 10-20% wheat protein aqueous solution, stirring and heating to 80-90 ℃ at a rotating speed of 200-260 r/min, adding 6-10% hydrochloric acid, wherein the volume ratio of the wheat protein aqueous solution to the hydrochloric acid is 1: (0.2-0.3), stirring and reacting for 5-6 hours at a rotating speed of 200-260 revolutions per minute; adjusting the pH value of the reaction solution to 6-7 by adopting a sodium hydroxide aqueous solution with the molar concentration of 0.1-0.2 mol/L; cooling the reaction liquid with the adjusted pH value to 20-30 ℃, adding activated carbon with the weight of 1-2% of the weight of the wheat protein, mixing, centrifuging at the rotating speed of 2000-3000 r/min for 10-15 min, and collecting supernatant; removing chloride ions contained in the supernatant, and drying for 10-16 hours at 50-55 ℃ and under the vacuum degree of 0.07-0.08 Mpa to obtain the acid hydrolysis wheat protein.

The acid hydrolysis of wheat protein has long reaction time, and is easy to cause the peptide chain of the protein to be broken, such as the tryptophan is completely destroyed, the serine and the tyrosine are partially destroyed, and components harmful to human bodies, such as dimethyl sulfide, methyl mercaptan, hydrogen sulfide, and the like, are produced. However, the reaction time is short, and the condition that the active peptide in the hydrolyzed wheat protein is low easily exists, so that the functionality of the hydrolyzed wheat protein is influenced.

The preparation process of the quaternized hydrolyzed wheat protein comprises the following steps:

(1) preparing a wheat protein aqueous solution with the mass fraction of 20-30%, stirring and heating the wheat protein aqueous solution to 45-50 ℃ at 200-260 r/min, adjusting the pH value of the wheat protein aqueous solution to 7.0-9.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1-0.2 mol/L, and stirring at the rotating speed of 200-260 r/min for 20-30 min to obtain a substrate solution; weighing protease which is 0.02-0.05 times of the weight of the wheat protein, adding the protease into a substrate solution, stirring and reacting for 1-4 hours at the rotating speed of 200-260 r/min, and adjusting the pH value of a reaction solution to be 7.0-9.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1-0.2 mol/L all the time in the reaction process; after the reaction is finished, regulating the pH value of the reaction solution to 6-7 by adopting hydrochloric acid with the mass fraction of 10-15%, and heating the reaction solution at 100 ℃ for 5-10 minutes to inactivate protease; cooling the reaction liquid to 20-25 ℃, adding activated carbon accounting for 1-2% of the weight of the wheat protein, mixing, centrifuging at the rotating speed of 2000-3000 r/min for 10-15 min, and collecting supernatant; drying the supernatant for 10-16 hours at 50-55 ℃ and under the vacuum degree of 0.07-0.08 Mpa to obtain hydrolyzed wheat protein;

(2) preparing hydrochloric acid with the molar concentration of 1-2 mol/L, adding dodecyl dimethyl tertiary amine with the molar concentration of 1-1.1 times of hydrogen chloride under the stirring condition of 230-260 revolutions/minute, heating to 50-55 ℃, adding epoxy chloropropane with the molar concentration of 0.95-0.99 times of the dodecyl dimethyl tertiary amine, and reacting for 3-4 hours to obtain reaction liquid A;

(3) cooling the reaction liquid A to 20-30 ℃, adjusting the pH value of the reaction liquid A to 10-11 by adopting a sodium hydroxide aqueous solution with the mass fraction of 20-25%, and stirring and reacting at the temperature of 20-30 ℃ at the rotating speed of 230-260 rpm for 2-3 hours to obtain a reaction liquid B;

(4) preparing a hydrolyzed wheat protein aqueous solution with the mass fraction of 10-15%, and adding the hydrolyzed wheat protein aqueous solution into the reaction liquid B, wherein the mass ratio of the hydrolyzed wheat protein aqueous solution to the reaction liquid B is (1.1-1.2): 1, heating to 65-70 ℃, stirring and reacting for 2-3 hours at a rotating speed of 230-260 revolutions per minute to obtain a reaction solution C;

(5) adjusting the pH value of the reaction liquid C to 5-7 by using citric acid, and concentrating the reaction liquid C for 4-5 hours at 50-60 ℃ under the vacuum degree of 0.06-0.07 MPa to obtain a crude product; washing the crude product by using an ethanol water solution with the volume fraction of 80-95%, wherein the solid-liquid ratio of the crude product to the ethanol water solution is 1 g: (50-100) mL, and drying for 6-8 hours at 40-50 ℃ and under the vacuum degree of 0.06-0.07 MPa to obtain the quaternized hydrolyzed wheat protein.

In the preparation process of the quaternized hydrolyzed wheat protein, the protease in the step (1) is one of trypsin, neutral protease and alkaline protease.

The quaternary ammonium salt has the characteristics of low irritation and compatibility with anions compared with other cationic conditioners, so that the quaternary ammonium salt hydrolyzed wheat protein has a better conditioning effect, the disheveled degree of hair is reduced, the dry combing property and the wet combing property are improved, and the smoothness of the hair surface is improved. The three proteases, trypsin, neutral protease and alkaline protease, have different action points. The content of arginine and lysine in the wheat protein is relatively low, so the enzymolysis degree of trypsin is not high; neutral protease mainly acts on hydrophobic amino acids, and the content of the hydrophobic amino acids such as proline and leucine in wheat protein is higher, so that the hydrolysis degree of the neutral protease is higher; alkaline protease has a relatively wide action on amino acids, so that alkaline protease has the highest degree of hydrolysis and the most sites suitable for quaternization reaction.

The wheat protein is treated by adopting amidase, deamidated, and functional characteristics such as emulsifying property, foaming property and the like of hydrolyzed wheat protein are provided, so that the application range of the hydrolyzed wheat protein is improved.

The preparation process of the amidase hydrolyzed wheat protein comprises the following steps: mixing wheat protein with a phosphate buffer solution with the pH of 7.0 and the molar concentration of 200mmol/L to obtain a dispersion liquid with the mass fraction of the wheat protein of 1-2%; stirring the dispersion liquid at a rotating speed of 200-260 rpm for 20-30 minutes, adding glutaminase with the mass of 0.02-0.05 time of that of the wheat protein, and performing enzymolysis for 10-15 hours at the temperature of 45-50 ℃ and the pH value of 7.3; after the reaction is finished, heating the reaction solution at 100 ℃ for 5-10 minutes to inactivate the glutaminase; cooling the reaction liquid to 20-25 ℃, adding activated carbon accounting for 1-2% of the weight of the wheat protein, mixing, centrifuging at the rotating speed of 2000-3000 r/min for 10-15 min, and collecting supernatant; and drying the supernatant for 10-16 hours at 50-55 ℃ and under the vacuum degree of 0.07-0.08 Mpa to obtain the amidase hydrolyzed wheat protein.

As a preferable technical scheme of the invention, the hydrolyzed wheat protein is a mixture of quaternized hydrolyzed wheat protein and amidase hydrolyzed wheat protein, wherein the mass ratio of the quaternized hydrolyzed wheat protein to the amidase hydrolyzed wheat protein is 1: 1.

The second technical problem to be solved by the invention is to provide a preparation method of special anti-hair loss shampoo for women.

The method for the special anti-hair loss shampoo for women comprises the following steps:

s1, adding 30-40 wt% of water, ammonium laureth sulfate, sodium lauroyl sarcosinate and EDTA disodium into preparation equipment, uniformly mixing, and heating to 80-85 ℃ to obtain a mixed solution I;

s2, adding ethylene glycol distearate, cetostearyl alcohol and methyl hydroxybenzoate into the mixed solution I, and uniformly mixing to obtain a mixed solution II;

s3, cooling the mixed solution II to 60-70 ℃, adding cocamidopropyl betaine, guar hydroxypropyl trimethyl ammonium chloride, panthenol and citric acid, and uniformly mixing to obtain a mixed solution III;

s4, cooling the mixed solution III to 45-50 ℃, adding the rest water, the cacumen biotae extract, the polygonum multiflorum root extract, the rhodiola rosea extract, the ginseng root extract and the ganoderma atrum extract, and uniformly mixing to obtain a mixed solution IV;

s5, cooling the mixed solution IV to 30-40 ℃, adding sodium chloride, hydrolyzed wheat protein, essence and methylisothiazolinone, and uniformly mixing to obtain a mixed solution V;

s6, standing the mixed solution V at 20-26 ℃ for 8-10 hours, and defoaming;

s7, quality inspection;

and S8, after the quality inspection is qualified, conveying the shampoo to a filling room, and filling according to a specified amount to obtain the special anti-hair loss shampoo for women.

The special anti-hair loss shampoo for women adopts beneficial natural substances, forms a protective film on the surface of hair through the skin and the surface layer of the hair, relieves stimulation, has the effects of smoothing pores, promoting hair growth and preventing hair loss, nourishing and moistening the hair, can effectively improve the scalp environment and promote the hair growth, and the hair is tough, moist, soft and refreshing after being washed by the shampoo.

Detailed Description

Introduction of raw materials in the examples:

ammonium laureth sulfate, CAS No.: 32612-48-9, available from JINNING BAICHUAN CHEMICAL CO.

Ammonium lauryl sulfate, CAS No.: 2235-54-3, available from Shanghai Cartesian Biotech Co., Ltd.

Cocamidopropyl betaine, CAS No.: 86438-79-1, available from Henan Tianfu chemical Co., Ltd.

Sodium lauroyl sarcosinate, CAS No.: 137-16-6, available from Guangdong Wengjiang chemical reagents, Inc.

Arborvitae, Latin school name: platycladus orientalis (L.) Franco, a evergreen arbor. Arborvitae was purchased from the breeding base of Linyi-Jumbo arborvitae.

Polygonum multiflorum, Latin scientific name: fallopia multiflora (Thunb.) Harald, also called wild seedling and Stephania japonica, is a perennial twisted vine of Polygonum genus of Polygonaceae family. Polygonum multiflorum is purchased from Michelia Hua agricultural product production and marketing professional cooperative.

Ethylene glycol distearate, CAS No.: 627-83-8, supplied by Shanghai di Bai Biotech limited.

Rhodiola rosea, Latin school name: rhodiola rosea l., alias: rhodiola rosea is a plant of perennial grass, wood or shrub of Crassulaceae. Rhodiola rosea is purchased from Xizangbuke drug development limited.

Ginseng, the scientific name of latin: panaxginseng, also known as Asian ginseng, is a fleshy root that is pharmaceutically acceptable. Ginseng is available from Gelmu Yuan Xintang Biotech Co., Ltd.

Guar hydroxypropyltrimonium chloride, CAS No.: 65497-29-2, supplied by Wuhan eosin science and technology, Inc.

Sodium chloride, CAS No.: 7647-14-5, available from chemical Co., Ltd, Waverrucke, Beijing.

The essence is lemon essence provided by Allen essence and spice Limited company.

Panthenol, CAS No.: 16485-10-2, available from Shandong Minye Chemicals, Inc.

Ganoderma atrum, Latin scientific name: ganoderma atrum, which is called the best product in Ganoderma, has the curative effect of medicinal Ganoderma atrum on human health care and can enhance the immune function of organisms. Black ganoderma is purchased from the cooperative society of natural ecological Chinese medicinal plant planting in Jinzhai county.

Cetostearyl alcohol, CAS No.: 67762-27-0, available from Vanda chemical Co., Ltd, Hangzhou.

Citric acid, CAS No.: 77-92-9, supplied by Wuhan Tian plant Biotechnology, Inc.

Disodium EDTA, CAS No.: 139-33-3, available from new chemical materials, inc.

Methylparaben, CAS number: 99-76-3, provided by Hangzhou Jie Chemicals, Inc.

Methylisothiazolinone, CAS No.: 2682-20-4, available from Guanyang chemical technology, Inc., Yangzhou.

Gelatin, CAS No.: 9000-70-8, available from Ranei Scutellaria of Nanjing Peng.

Glutinous rice was purchased from Xiamen Changsheng grain and oil Co.

Distiller's yeast, purchased from south ochre commerce ltd.

Preparing yeast wine: mixing glutinous rice and water in a mass ratio of 1:10, soaking for 8 hours at 25 ℃, taking out, draining, wrapping with gauze, and then putting into a steamer to steam for 40 minutes at 100 ℃; then taking out glutinous rice, spreading and cooling to 30 ℃, adding water 1.5 times of the weight of the glutinous rice, then adding distiller's yeast 3% of the weight of the glutinous rice and yeast 0.3% of the weight of the glutinous rice (food grade provided by Shandong Sheng biological science and technology Co., Ltd.), mixing uniformly, and culturing at 24 ℃ for 8 hours to obtain the yeast.

Wheat protein, purchased from Shandong Jianchuan Biotech limited.

The activated carbon is coconut shell activated carbon provided by Wuxi Bei Zhan environmental protection science and technology limited.

Dodecyl dimethyl tertiary amine, CAS No.: CAS:112-18-5, available from Bailingwei technologies, Inc.

Epichlorohydrin, CAS No.: 106-89-8, supplied by Meilanjia Kogyo (Shanghai) Co., Ltd.

Citric acid, CAS No.: 77-92-9, provided by the chemical company of the silver river, Hubei.

Trypsin, purchased from baiwei biotechnology limited, hebei, with an enzyme activity of 20U/g.

The neutral protease is 1398 type neutral protease provided by Nanning Dong Henghuadao biotechnology Limited liability company, and is prepared by culturing and fermenting Bacillus subtilis, and refining by biotechnology, and the enzyme activity is 20U/g.

The alkaline protease is 2709 alkaline protease provided by Nanning Dong Henghuadao bioscience Limited liability company, is proteolytic enzyme prepared by fermenting and extracting Bacillus licheniformis, and has the main component of Bacillus licheniformis protease and the enzyme activity of 20U/g.

A phosphate buffer solution having a pH of 7.0 and a molar concentration of 200mmol/L was prepared by mixing 61ml of 0.2mol/L disodium hydrogenphosphate and 39ml of 0.2mol/L sodium dihydrogenphosphate.

Glutaminase is provided by Pengpo bioengineering company of Nanning, and the enzyme activity is 100U/g.

Example 1

The anti-hair loss shampoo special for women has the following formula: 9 wt% of ammonium laureth sulfate, 5 wt% of cocamidopropyl betaine, 2 wt% of sodium lauroyl sarcosinate, 1.2 wt% of cacumen biotae extract, 1.2 wt% of polygonum multiflorum root extract, 1.2 wt% of ethylene glycol distearate, 0.7 wt% of rhodiola rosea extract, 0.7 wt% of ginseng root extract, 0.5 wt% of guar hydroxypropyltrimonium chloride, 0.5 wt% of sodium chloride, 0.5 wt% of acid hydrolyzed wheat protein, 0.5 wt% of essence, 0.3 wt% of panthenol, 0.3 wt% of ganoderma atrum extract, 0.3 wt% of cetearyl alcohol, 0.15 wt% of citric acid, 0.1 wt% of disodium EDTA, 0.1 wt% of methylparaben, 0.05 wt% of methylisothiazolinone, and the balance of water.

The preparation process of the cacumen biotae extract comprises the following steps: pulverizing folium Platycladi, and sieving with 80 mesh sieve to obtain folium Platycladi powder; mixing cacumen biotae powder and 70% by volume of ethanol aqueous solution in a material-liquid ratio of 1: 25(g/mL), and extracting at 80 deg.C for 3 hr to obtain folium Platycladi extract; adding a gelatin aqueous solution with the mass fraction of 2% into the cacumen biotae extracting solution, wherein the volume ratio of the cacumen biotae extracting solution to the gelatin aqueous solution is 1: 0.12, standing for 12 hours at 23 ℃ after uniformly mixing, filtering by adopting 100-mesh filter cloth, and collecting filtrate; drying the filtrate at 50 deg.C under vacuum degree of 0.08MPa for 10 hr to obtain the folium Platycladi extract.

The preparation of the polygonum multiflorum root extract, the rhodiola rosea extract, the ginseng root extract and the ganoderma atrum extract is carried out with reference to the preparation of the cacumen biotae extract, and the cacumen biotae is replaced by polygonum multiflorum root, rhodiola rosea, ginseng root and ganoderma atrum respectively to obtain the polygonum multiflorum root extract, the rhodiola rosea extract, the ginseng root extract and the ganoderma atrum extract.

The preparation process of the acid hydrolysis wheat protein comprises the following steps: preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating to 90 ℃ at the rotating speed of 260 revolutions per minute, adding hydrochloric acid with the mass fraction of 10%, wherein the volume ratio of the wheat protein aqueous solution to the hydrochloric acid is 1: 0.2, stirring and reacting for 5 hours at the rotating speed of 260 revolutions per minute; adjusting the pH value of the reaction solution to 7 by adopting a sodium hydroxide aqueous solution with the molar concentration of 0.1 mol/L; cooling the reaction solution with the adjusted pH value to 25 ℃, adding activated carbon with the weight of 2% of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; removing chloride ions contained in the supernatant, and drying at 50 deg.C and 0.07Mpa for 12 hr to obtain the acid hydrolyzed wheat protein.

The preparation method of the special anti-hair loss shampoo for women comprises the following steps:

s1, adding 30 wt% of water, ammonium laureth sulfate, sodium lauroyl sarcosinate and disodium EDTA into a preparation device, uniformly mixing, and heating to 80 ℃ to obtain a mixed solution I;

s3, cooling the mixed solution II to 70 ℃, adding cocamidopropyl betaine, guar hydroxypropyl trimonium chloride, panthenol and citric acid, and uniformly mixing to obtain a mixed solution III;

s4, cooling the mixed solution III to 50 ℃, adding the rest water, the cacumen biotae extract, the polygonum multiflorum root extract, the rhodiola rosea extract, the ginseng root extract and the ganoderma atrum extract, and uniformly mixing to obtain a mixed solution IV;

s5, cooling the mixed solution IV to 40 ℃, adding sodium chloride, acid hydrolysis wheat protein, essence and methylisothiazolinone, and uniformly mixing to obtain a mixed solution V;

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Example 2

The preparation process of the ginseng root extract comprises the following steps: pulverizing Ginseng radix, and sieving with 80 mesh sieve to obtain Ginseng radix powder; cleaning glutinous rice, adding water 10 times of glutinous rice weight, soaking for 8 hr, taking out, draining, wrapping with gauze, steaming in a steamer at 100 deg.C for 30 min, taking out, and placing into a fermentation device; adding radix Ginseng powder, water, yeast and yeast into a fermentation device, wherein the addition amounts of radix Ginseng powder, water, yeast and yeast are 30%, 1.5%, 2% and 0.3% of the weight of Oryza Glutinosa respectively, mixing well, and fermenting at 17 deg.C for 20 days; after fermentation is finished, filtering a fermentation product by using 100-mesh filter cloth, and collecting filtrate; drying the filtrate at 50 deg.C under vacuum degree of 0.08MPa for 10 hr to obtain Ginseng radix extract.

HPLC conditions: a chromatographic column: BDS HYPERSIL C18 column (250 mm. times.4.6 mm, 5 μm); column temperature: at 25 ℃. Detection wavelength: 203 nm. Mobile phase: water (a) and acetonitrile (B); flow rate: 1.0 mL/min.

The content of ginsenoside in the ginseng root extract is detected by an HPLC method, and the result shows that the content of ginsenoside in example 2 is obviously higher than that in example 1, and rare ginsenoside which does not appear in example 1 is detected. This indicates that the content of ginsenoside is increased under the action of distiller's yeast and yeast, and that the common saponin in ginseng is converted to form more functional rare ginsenoside, which enhances the functionality of ginseng extract. In addition, the cytotoxicity of the ginseng root extract is detected by adopting an MTT method, and the result shows that the ginseng root extract has no cytotoxicity.

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Example 3

The anti-hair loss shampoo special for women has the following formula: 9 wt% of ammonium laureth sulfate, 5 wt% of cocamidopropyl betaine, 2 wt% of sodium lauroyl sarcosinate, 1.2 wt% of cacumen biotae extract, 1.2 wt% of polygonum multiflorum root extract, 1.2 wt% of ethylene glycol distearate, 0.7 wt% of rhodiola rosea extract, 0.7 wt% of ginseng root extract, 0.5 wt% of guar hydroxypropyltrimonium chloride, 0.5 wt% of sodium chloride, 0.5 wt% of quaternized hydrolyzed wheat protein, 0.5 wt% of essence, 0.3 wt% of panthenol, 0.3 wt% of ganoderma atrum extract, 0.3 wt% of cetearyl alcohol, 0.15 wt% of citric acid, 0.1 wt% of disodium EDTA, 0.1 wt% of methylparaben, 0.05 wt% of methylisothiazolinone, and the balance of water.

(1) preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating the wheat protein aqueous solution to 50 ℃ at 260 revolutions per minute, adjusting the pH value of the wheat protein aqueous solution to 8.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L, and stirring at the rotating speed of 260 revolutions per minute for 30 minutes to obtain a substrate solution; weighing trypsin which is 0.03 time of the weight of the wheat protein, adding the trypsin into a substrate solution, stirring and reacting for 3 hours at the rotating speed of 260 r/min, and always adjusting the pH value of a reaction solution to be 8.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L in the reaction process; after the reaction is finished, hydrochloric acid with the mass fraction of 15% is adopted to adjust the pH value of the reaction solution to 7, and the reaction solution is heated at 100 ℃ for 10 minutes to inactivate trypsin; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; drying the supernatant at 50 deg.C under 0.07Mpa for 12 hr to obtain hydrolyzed wheat protein;

(2) preparing hydrochloric acid with the molar concentration of 1.5mol/L, adding dodecyl dimethyl tertiary amine with the molar concentration of 1.1 times of hydrogen chloride under the stirring condition of 260 revolutions per minute, heating to 50 ℃, adding epoxy chloropropane with the molar concentration of 0.99 times of the dodecyl dimethyl tertiary amine, and reacting for 4 hours to obtain reaction liquid A;

(3) cooling the reaction liquid A to 25 ℃, adjusting the pH value of the reaction liquid A to 11 by adopting a sodium hydroxide aqueous solution with the mass fraction of 20%, and stirring and reacting for 2 hours at the temperature of 25 ℃ at the rotating speed of 260 revolutions per minute to obtain a reaction liquid B;

(4) preparing a hydrolyzed wheat protein aqueous solution with the mass fraction of 10%, and adding the hydrolyzed wheat protein aqueous solution into the reaction liquid B, wherein the mass ratio of the hydrolyzed wheat protein aqueous solution to the reaction liquid B is 1.2: 1, heating to 70 ℃, and stirring at the rotating speed of 260 revolutions per minute for reaction for 3 hours to obtain a reaction solution C;

(5) adjusting the pH value of the reaction solution C to 6 by using citric acid, and concentrating the reaction solution C for 4 hours at the temperature of 50 ℃ and the vacuum degree of 0.07MPa to obtain a crude product; washing the crude product by using an ethanol water solution with the volume fraction of 90%, wherein the solid-liquid ratio of the crude product to the ethanol water solution is 1: 80(g/mL), and drying for 8 hours at 50 ℃ and under the vacuum degree of 0.07MPa to obtain the quaternized hydrolyzed wheat protein.

s5, cooling the mixed solution IV to 40 ℃, adding sodium chloride, quaternized hydrolyzed wheat protein, essence and methylisothiazolinone, and uniformly mixing to obtain a mixed solution V;

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Example 4

(1) preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating the wheat protein aqueous solution to 50 ℃ at 260 revolutions per minute, adjusting the pH value of the wheat protein aqueous solution to 7.0 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L, and stirring at the rotating speed of 260 revolutions per minute for 30 minutes to obtain a substrate solution; weighing neutral protease with the weight 0.03 time of that of the wheat protein, adding the neutral protease into a substrate solution, stirring and reacting for 3 hours at the rotating speed of 260 r/min, and always adjusting the pH value of a reaction solution to be 7.0 by adopting a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L in the reaction process; after the reaction is finished, hydrochloric acid with the mass fraction of 15% is adopted to adjust the pH value of the reaction solution to 7, and the reaction solution is heated at 100 ℃ for 10 minutes to inactivate neutral protease; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; drying the supernatant at 50 deg.C under 0.07Mpa for 12 hr to obtain hydrolyzed wheat protein;

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Example 5

(1) preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating the wheat protein aqueous solution to 50 ℃ at 260 revolutions per minute, adjusting the pH value of the wheat protein aqueous solution to 9.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L, and stirring at the rotating speed of 260 revolutions per minute for 30 minutes to obtain a substrate solution; weighing alkaline protease with the weight 0.03 time of that of the wheat protein, adding the alkaline protease into a substrate solution, stirring and reacting for 3 hours at the rotating speed of 260 r/min, and always adjusting the pH value of a reaction solution to be 9.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L in the reaction process; after the reaction is finished, hydrochloric acid with the mass fraction of 15% is adopted to adjust the pH value of the reaction liquid to 7, and the reaction liquid is heated at 100 ℃ for 10 minutes to inactivate alkaline protease; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; drying the supernatant at 50 deg.C under 0.07Mpa for 12 hr to obtain hydrolyzed wheat protein;

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Example 6

The anti-hair loss shampoo special for women has the following formula: 9 wt% of ammonium laureth sulfate, 5 wt% of cocamidopropyl betaine, 2 wt% of sodium lauroyl sarcosinate, 1.2 wt% of cacumen biotae extract, 1.2 wt% of polygonum multiflorum root extract, 1.2 wt% of ethylene glycol distearate, 0.7 wt% of rhodiola rosea extract, 0.7 wt% of ginseng root extract, 0.5 wt% of guar hydroxypropyltrimonium chloride, 0.5 wt% of sodium chloride, 0.5 wt% of amidase hydrolyzed wheat protein, 0.5 wt% of essence, 0.3 wt% of panthenol, 0.3 wt% of ganoderma atrum extract, 0.3 wt% of cetearyl alcohol, 0.15 wt% of citric acid, 0.1 wt% of disodium EDTA, 0.1 wt% of methylparaben, 0.05 wt% of methylisothiazolinone, and the balance of water.

The preparation process of the amidase hydrolyzed wheat protein comprises the following steps: mixing wheat protein with phosphate buffer solution with pH of 7.0 and molar concentration of 200mmol/L to obtain dispersion liquid with wheat protein mass fraction of 2%; stirring the dispersion liquid at the rotating speed of 260 r/min for 30 min, adding glutaminase with the mass of 0.03 time of the wheat protein, and carrying out enzymolysis for 12 h at the temperature of 45 ℃ and the pH value of 7.3; after the reaction, the reaction solution was heated at 100 ℃ for 10 minutes to inactivate glutaminase; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; and drying the supernatant for 12 hours at the temperature of 50 ℃ and the vacuum degree of 0.07Mpa to obtain the amidase hydrolyzed wheat protein.

s5, cooling the mixed solution IV to 40 ℃, adding sodium chloride, amidase hydrolyzed wheat protein, essence and methylisothiazolinone, and uniformly mixing to obtain a mixed solution V;

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Example 7

The anti-hair loss shampoo special for women has the following formula: 9 wt% of ammonium laureth sulfate, 5 wt% of cocamidopropyl betaine, 2 wt% of sodium lauroyl sarcosinate, 1.2 wt% of cacumen biotae extract, 1.2 wt% of polygonum multiflorum root extract, 1.2 wt% of ethylene glycol distearate, 0.7 wt% of rhodiola rosea extract, 0.7 wt% of ginseng root extract, 0.5 wt% of guar hydroxypropyltrimonium chloride, 0.5 wt% of sodium chloride, 0.25 wt% of quaternized hydrolyzed wheat protein, 0.25 wt% of amidase hydrolyzed wheat protein, 0.5 wt% of essence, 0.3 wt% of panthenol, 0.3 wt% of ganoderma atrum extract, 0.3 wt% of cetearyl alcohol, 0.15 wt% of citric acid, 0.1 wt% of disodium EDTA, 0.1 wt% of methylparaben, 0.05 wt% of methylisothiazolinone, and the balance of water.

s5, cooling the mixed solution IV to 40 ℃, adding sodium chloride, quaternized hydrolyzed wheat protein, amidase hydrolyzed wheat protein, essence and methylisothiazolinone, and uniformly mixing to obtain a mixed solution V;

s6, standing the mixed solution V at 25 ℃ for 8 hours, and defoaming;

s7, quality inspection;

Test example 1

The anti-hair loss shampoo for women of example 1 was subjected to performance test:

80 female subjects with alopecia symptoms are 18-65 years old. The using method comprises the following steps: the special anti-hair loss shampoo for women is directly used by a test subject once every other day, the hair is wetted before use, a proper amount of the embodiment is squeezed out of the palm, the hair is directly smeared on the palm, rich foam is kneaded, and the scalp is massaged for about 3 minutes by using the palm, and then the hair is washed clean by using clear water. After the persistent use for one month, the hair of 68 subjects became soft and black, and the hair loss was improved.

Test example 2

The total flavone content, total flavone content and antioxidant activity of the ginseng root extracts of examples 1-2 were measured, respectively.

And (3) total phenol content determination: drawing a tannic acid standard curve: 0.5mL of tannic acid solution with different concentrations is taken, 0.5mL of 10% Folin-Ciocalteu solution is added, 0.4mL of sodium carbonate solution with the mass fraction of 7.5% is added after uniform mixing, reaction is carried out for 30 minutes at room temperature after uniform mixing, and then the absorbance is measured at 750nm and a standard curve is drawn. Determination of ginseng root extract: the procedure was the same as for the tannic acid standard curve, except that the tannic acid solution was replaced with a sample solution having a concentration of 1 mg/mL. The phenol content was calculated according to the linear regression equation and the test results were in terms of tannic acid (mg/g).

And (3) total flavone content determination: drawing a rutin standard curve: taking 1mL of rutin solution with different concentrations, adding 0.1mL of 10% aluminum trichloride solution and 0.1mL of 1mol/L potassium acetate solution respectively, uniformly mixing, adding 2.8mL of distilled water and 1mL of 95% ethanol by volume fraction, reacting for 40 minutes at room temperature after uniformly mixing, and then measuring absorbance at 415nm and drawing a standard curve. Determination of ginseng root extract: the operation method is the same as that of drawing a rutin standard curve, and only the rutin solution is replaced into a sample solution with the concentration of 1 mg/mL. The phenol content was calculated according to the linear regression equation and the test results were in terms of rutin (mg/g).

Determination of antioxidant Activity: taking 0.02mL of ginseng root extract solution with different concentrations, adding 0.02mL of sulfuric acid with the molar concentration of 0.6mol/L, continuously adding 0.2mL of 28mmol/L sodium phosphate solution and 0.2mL of 4mmol/L sodium molybdate solution respectively after uniformly mixing, placing in a water bath kettle at 95 ℃ after uniformly mixing, reacting for 90 minutes, taking out, cooling and determining the absorbance at 685 nm. BHA was used as a control.

The specific test results are shown in table 1.

Table 1: performance test result table of ginseng root extract

As can be seen from table 1, the total phenol and total flavone contents of the ginseng root extract in example 2 are significantly higher than those in example 1, and the antioxidant activity is also significantly enhanced, presumably because a large amount of functional components existing in ginseng during fermentation are fully dissolved in the fermentation broth, and common saponins in ginseng are converted into more functional rare ginsenosides by fermentation.

Test example 3

The performance of the hydrolyzed wheat proteins used in examples 2-7 was tested.

Foaming capacity was determined by the Ross-Miles method, reference GB/T7462-87: respectively adopting deionized water to prepare hydrolyzed wheat protein or quaternized hydrolyzed wheat protein into 0.6 mass percent solution, adjusting the pH of the solution to 7 by using 20 mass percent sodium hydroxide aqueous solution, and then measuring the foaming capacity of the hydrolyzed protein solution.

Adsorption test: the method comprises the following steps of arranging hair into hair bundles with the weight of 2g per bundle, soaking the hair bundles in 5% hydrolyzed wheat protein aqueous solution for 30 minutes, cleaning the hair bundles with clear water, naturally airing the hair bundles, and measuring the weight gain of the hair bundles.

The specific test results are shown in table 2.

Table 2: test result table for performance of hydrolyzed wheat protein or quaternized hydrolyzed wheat protein

As can be seen from Table 2, although the wheat proteins were hydrolyzed by acid in examples 1 to 2, the peptide chains of the proteins were easily broken due to the long time of hydrolysis, and the amino acid structures were changed to generate harmful components to the human body. Therefore, the time for acid hydrolysis is controlled in the invention, so that the hydrolysis reaction is incomplete, and the functionality of the hydrolyzed wheat protein is influenced to a certain extent. Examples 3 to 5 used quaternized hydrolyzed proteins having opsonizability of natural materials such as proteins and having adsorbability of quaternary ammonium salts. By introducing quaternary ammonium ions into the tail end of the hydrolyzed wheat protein, the isoelectric point of high protein is provided, and the adsorbability of the protein to hair is increased, so that the adhesiveness of the quaternized wheat hydrolyzed protein is superior to that of the hydrolyzed wheat protein, the quaternized wheat hydrolyzed protein can provide stronger conditioning capability than the hydrolyzed protein, and the quaternized wheat hydrolyzed protein has more obvious effects on improving static accumulation, smoothing hair and the like.

Claims

1. A method for preparing quaternized hydrolyzed wheat protein comprises the following steps:

(1) providing hydrolyzed wheat protein, the method of making the hydrolyzed wheat protein comprising:

preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating the wheat protein aqueous solution to 50 ℃ at 260 revolutions per minute, adjusting the pH value of the wheat protein aqueous solution to 8.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L, and stirring at the rotating speed of 260 revolutions per minute for 30 minutes to obtain a substrate solution; weighing trypsin which is 0.03 time of the weight of the wheat protein, adding the trypsin into a substrate solution, stirring and reacting for 3 hours at the rotating speed of 260 r/min, and always adjusting the pH value of a reaction solution to be 8.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L in the reaction process; after the reaction is finished, hydrochloric acid with the mass fraction of 15% is adopted to adjust the pH value of the reaction solution to 7, and the reaction solution is heated at 100 ℃ for 10 minutes to inactivate trypsin; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; drying the supernatant at 50 deg.C under 0.07Mpa for 12 hr to obtain hydrolyzed wheat protein;

or preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating the wheat protein aqueous solution to 50 ℃ at 260 revolutions per minute, adjusting the pH value of the wheat protein aqueous solution to 7.0 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L, and stirring at the rotating speed of 260 revolutions per minute for 30 minutes to obtain a substrate solution; weighing neutral protease with the weight 0.03 time of that of the wheat protein, adding the neutral protease into a substrate solution, stirring and reacting for 3 hours at the rotating speed of 260 r/min, and always adjusting the pH value of a reaction solution to be 7.0 by adopting a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L in the reaction process; after the reaction is finished, hydrochloric acid with the mass fraction of 15% is adopted to adjust the pH value of the reaction solution to 7, and the reaction solution is heated at 100 ℃ for 10 minutes to inactivate neutral protease; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; drying the supernatant at 50 deg.C under 0.07Mpa for 12 hr to obtain hydrolyzed wheat protein;

or preparing a wheat protein aqueous solution with the mass fraction of 20%, stirring and heating the wheat protein aqueous solution to 50 ℃ at 260 revolutions per minute, adjusting the pH value of the wheat protein aqueous solution to 9.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L, and stirring at the rotation speed of 260 revolutions per minute for 30 minutes to obtain a substrate solution; weighing alkaline protease with the weight 0.03 time of that of the wheat protein, adding the alkaline protease into a substrate solution, stirring and reacting for 3 hours at the rotating speed of 260 r/min, and always adjusting the pH value of a reaction solution to be 9.5 by using a sodium hydroxide aqueous solution with the molar concentration of 0.1mol/L in the reaction process; after the reaction is finished, hydrochloric acid with the mass fraction of 15% is adopted to adjust the pH value of the reaction liquid to 7, and the reaction liquid is heated at 100 ℃ for 10 minutes to inactivate alkaline protease; cooling the reaction liquid to 25 ℃, adding activated carbon with the weight of 2% of the weight of the wheat protein, mixing, centrifuging for 15 minutes at the rotating speed of 3000 r/min, and collecting supernatant; drying the supernatant at 50 deg.C under 0.07Mpa for 12 hr to obtain hydrolyzed wheat protein;

(4) preparing 10% of the aqueous solution of the hydrolyzed wheat protein in the step (1), and adding the aqueous solution of the hydrolyzed wheat protein into the reaction liquid B, wherein the mass ratio of the aqueous solution of the hydrolyzed wheat protein to the reaction liquid B is 1.2: 1, heating to 70 ℃, and stirring at the rotating speed of 260 revolutions per minute for reaction for 3 hours to obtain a reaction solution C;

(5) adjusting the pH value of the reaction solution C to 6 by using citric acid, and concentrating the reaction solution C for 4 hours at 50 ℃ and under the vacuum degree of 0.07MPa to obtain a crude product; washing the crude product by using an ethanol water solution with the volume fraction of 90%, wherein the solid-liquid ratio of the crude product to the ethanol water solution is 1: 80(g/mL), and drying for 8 hours at 50 ℃ and under the vacuum degree of 0.07MPa to obtain the quaternized hydrolyzed wheat protein.

2. The use of the quaternized hydrolyzed wheat protein prepared by the preparation method of claim 1 in the preparation of anti-hair loss shampoo for women.

3. The use according to claim 2, wherein said lady specific anti-hair loss shampoo comprises a lady specific anti-hair loss shampoo to improve static electricity accumulation and/or a lady specific anti-hair loss shampoo to smooth hair.