CN113855588A - Method for preparing keratin solution by wool hydrolysis - Google Patents

Method for preparing keratin solution by wool hydrolysis Download PDF

Info

Publication number
CN113855588A
CN113855588A CN202111352548.9A CN202111352548A CN113855588A CN 113855588 A CN113855588 A CN 113855588A CN 202111352548 A CN202111352548 A CN 202111352548A CN 113855588 A CN113855588 A CN 113855588A
Authority
CN
China
Prior art keywords
wool
solution
keratin
enzymolysis
hydrolysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111352548.9A
Other languages
Chinese (zh)
Inventor
杨瑞强
王晓莉
诸冬寒
刘新贵
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Weizhixin Biotechnology Co ltd
Original Assignee
Shanghai Weizhixin Biotechnology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Weizhixin Biotechnology Co ltd filed Critical Shanghai Weizhixin Biotechnology Co ltd
Priority to CN202111352548.9A priority Critical patent/CN113855588A/en
Publication of CN113855588A publication Critical patent/CN113855588A/en
Pending legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/65Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P21/00Preparation of peptides or proteins
    • C12P21/06Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Zoology (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Molecular Biology (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Biotechnology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • Genetics & Genomics (AREA)
  • Dermatology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a method for preparing keratin solution by hydrolyzing wool, which comprises the steps of firstly soaking wool in acid solution with certain mass percentage concentration, heating for softening, cooling, washing with water and drying to obtain acidified wool; adding the obtained acidified wool into water, dropwise adding alkali liquor under an ultrasonic condition to adjust the pH value to 8.0-10.5, and filtering; carrying out enzymolysis on the pretreated wool by using subtilisin, inactivating enzyme after the enzymolysis is finished, adding activated carbon for decolorization, and filtering to obtain a hydrolyzed wool keratin dilute solution; and (3) concentrating the dilute hydrolyzed wool keratin solution on a concentrating device to obtain a hydrolyzed keratin solution. The acidification pretreatment in the method reduces the hardness of wool keratin, reduces the difficulty of wool enzymolysis, improves the wool enzymolysis efficiency and reduces the molecular weight of hydrolyzed keratin. The invention has simple process and convenient operation, the wool dissolution rate of the invention can reach more than 70 percent, and the extraction rate can reach more than 60 percent.

Description

Method for preparing keratin solution by wool hydrolysis
Technical Field
The invention belongs to the technical field of keratin preparation methods, and particularly relates to a method for preparing a keratin solution by wool hydrolysis.
Background
Wool contains more than 80% of alpha-keratin, the structure of the alpha-keratin has high similarity with keratin in human hair, and the wool is hydrolyzed to prepare low molecular weight hydrolyzed keratin which can be used as a hair conditioner to be applied to hair washing and protecting products. Because the keratin molecular structure contains a large number of disulfide bonds, the crosslinking is generated inside the peptide chain and among the peptide chains, and a stable three-dimensional network structure is formed, so that the degradation of the keratin macromolecules has certain difficulty. At present, the wool dissolving method mainly comprises a mechanical method, an oxidation method, a reduction method, an acid-base method, a metal salt method, a copper ammonia solution method and the like. Researches show that the methods have certain defects, such as excessive molecular weight, low degradation rate, poor product purity, color, smell and stability and the like, and the obtained products cannot be applied to cosmetics. The enzymolysis method is characterized in that specific biological enzyme is utilized to break specific chemical bonds in protein molecular chains so as to prepare protein hydrolysate, the enzymolysis condition is mild, certain specificity is realized, side reactions are few, and the obtained protein hydrolysate is uniform in composition and is the best way for preparing small-molecule protein hydrolysate. Chinese invention patent CN109689022A describes a low molecular weight keratin hydrolysate, which is prepared by performing oxidation pretreatment of keratin, then performing enzymolysis under the hydrolysis action of endopeptidase and exopeptidase respectively to obtain keratin hydrolysate with molecular weight below 1000Da, and applying the keratin hydrolysate as a conditioner to skin and hair cleaning products.
Disclosure of Invention
The invention provides a method for preparing a keratin solution by hydrolyzing wool in order to overcome the defects in the prior art.
The invention is realized by the following technical scheme: the invention discloses a method for preparing a keratin solution by wool hydrolysis, which comprises the following steps:
(1) soaking wool in an acid solution with a certain mass percentage concentration, heating for softening, cooling, washing with water, and drying to obtain acidified wool;
(2) adding the acidified wool obtained in the step (1) into water, dropwise adding alkali liquor under an ultrasonic condition to adjust the pH value to 8.0-10.5, and filtering;
(3) carrying out enzymolysis on the pretreated wool obtained in the step (2) by using subtilisin, inactivating enzyme after the enzymolysis is finished, adding activated carbon for decolorization, and filtering to obtain a hydrolyzed wool keratin dilute solution;
(4) and (4) filtering and concentrating the dilute hydrolyzed wool keratin solution obtained in the step (3) on a concentrating device to obtain a hydrolyzed keratin solution.
Preferably, the length of the wool in the step (1) is controlled to be less than 5cm, the acid solution is one or more of acetic acid, oxalic acid, citric acid, hydrochloric acid, sulfuric acid or lactic acid, and the mass percentage concentration of the acid solution is 3-15%.
Preferably, in the step (1), wool and the acid solution are mixed according to a mass ratio of 1: feeding materials at a ratio of 5-1: 20, treating for 4-24 hours at a temperature of 60-90 ℃, and drying after cooling and water washing.
Preferably, the alkali liquor in step (2) is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium sulfite or sodium bisulfite.
Preferably, the mass percentage of the subtilisin in the acidified wool solution in the step (3) is 0.1-15%; the temperature of the enzymolysis step is 40-75 ℃, the enzymolysis PH = 8.0-10.5, the enzymolysis time is 16-72 h, and the enzyme deactivation condition is heat preservation treatment for 0.5-2 h under the temperature condition of 70-90 ℃; the mass ratio of the active carbon to the enzymolysis solution is (0.1-1): 100, the decoloring temperature is 60-90 ℃, and the decoloring time is 0.5-4 h.
As the best embodiment of the invention, the temperature of the enzymolysis step in the step (3) is 45 ℃, the enzymolysis pH =10, the enzymolysis time is 36h, and the enzyme deactivation condition is heat preservation treatment for 1h under the condition of 80 ℃; the mass ratio of the active carbon to the enzymolysis solution is 1:100, the decoloring temperature is 80 ℃, and the decoloring time is 1.5 h.
The hydrolyzed keratin solution in the step (4) is a clear and transparent yellow solution or a light yellow solution, the mass percentage is more than 18 percent, and the molecular weight is 500Da to 2000 Da.
The invention has the beneficial effects that: the invention aims to provide a method for preparing a keratin solution by wool hydrolysis, and the obtained product can be used as a hair conditioner, enters the interior of hair by means of permeation and surface adsorption and forms a protective film on the surface of the hair so as to improve the problems of hair damage, hair dryness and the like. Generally, the lower the molecular weight of the protein hydrolysate, the better the permeability, but not the film formation; in contrast, protein hydrolysates with a high molecular weight have good film forming properties but poor permeability. In order to fully exert the repairing function of protein hydrolysate from inside to outside, the invention takes wool as raw material, and hydrolyzes the wool according to the processes of acidification pretreatment, primary enzymolysis, decoloration, membrane separation and the like to prepare the low molecular weight keratin solution.
The acidification pretreatment in the method for preparing the keratin solution by hydrolyzing wool reduces the hardness of wool keratin, reduces the difficulty of wool enzymolysis, improves the wool enzymolysis efficiency and reduces the molecular weight of the hydrolyzed keratin. The method for preparing the keratin solution by hydrolyzing the wool has simple process and convenient operation, the wool dissolution rate of the invention can reach more than 70 percent, the extraction rate can reach more than 60 percent, the hydrolysis degree is high, the molecular weight of the obtained keratin is mainly concentrated in 500 Da-2000 Da, the permeability of the keratin in hair is ensured, and better film-forming property is provided.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1:
(1) soaking 20g of wool in 100g of sulfuric acid solution with the mass fraction of 3%, preserving heat at 90 ℃ for 4h, cooling to room temperature, filtering to remove acid solution, leaching with 500g of deionized water, and drying to obtain acidified wool;
(2) putting the wool obtained in the step (1) into 100g of deionized water, and slowly adding Na with the concentration of 0.5% dropwise under the ultrasonic condition2CO3Adjusting the pH value of the solution to be about 10.0, and filtering;
(3) heating to 45 ℃, adjusting the pH =10.0, adding subtilisin with the mass percent of acidified wool being 15% for enzymolysis, keeping the pH at about 10.0 for enzymolysis for 16h, inactivating enzyme after the enzymolysis is finished, heating to 90 ℃ and maintaining for 0.5 h;
(4) adding 1g of activated carbon into the step (3), stirring and decoloring for 0.5h at the temperature of 90 ℃, and filtering after decoloring to obtain a light yellow clear hydrolyzed keratin solution;
(5) purifying and concentrating the hydrolyzed keratin solution obtained in the step (4) by a membrane separation technology to obtain a yellow transparent keratin solution with the mass fraction of more than 18% and the molecular weight of 500 Da-2000 Da.
Example 2:
(1) soaking 10g of wool in 100g of 10% hydrochloric acid solution, preserving heat at 70 ℃ for 12h, cooling to room temperature, filtering to remove the acid solution, leaching with 500g of deionized water, and drying to obtain acidified wool;
(2) putting the wool obtained in the step (1) into 100g of deionized water, slowly dropwise adding NaOH with the concentration of 0.2% under an ultrasonic condition, adjusting the pH value of the solution to be about 9.5, and filtering;
(3) heating to 55 ℃, adjusting the pH =9.5, adding subtilisin with the mass percent of acidified wool being 10% for enzymolysis, keeping the pH at about 9.5 for enzymolysis for 48h, inactivating enzyme after the enzymolysis is finished, heating to 80 ℃ and maintaining for 1 h;
(4) adding 0.7g of activated carbon into the step (3), stirring and decoloring for 2h at the temperature of 80 ℃, and filtering after decoloring to obtain a light yellow clear hydrolyzed keratin solution;
(5) purifying and concentrating the hydrolyzed keratin solution obtained in the step (4) by a membrane separation technology to obtain a yellow transparent keratin solution with the mass fraction of 18% and the molecular weight of 500 Da-2000 Da.
Example 3:
(1) soaking 5g of wool in 100g of acetic acid solution with the mass fraction of 15%, preserving heat at 60 ℃ for 24h, cooling to room temperature, filtering to remove the acid solution, leaching with 500g of deionized water, and drying to obtain acidified wool;
(2) putting the wool obtained in the step (1) into 100g of deionized water, slowly dropwise adding KOH with the concentration of 0.5% under the ultrasonic condition, adjusting the pH of the solution to be about 8, and filtering;
(3) heating to 75 ℃, adjusting the pH =8, adding subtilisin with the mass percent of acidified wool being 1.5% for enzymolysis, keeping the pH at about 8 for enzymolysis for 72h, inactivating enzyme after the enzymolysis is finished, heating to 70 ℃ and maintaining for 2 h;
(4) adding 0.1g of activated carbon into the step (3), stirring and decoloring for 4 hours at the temperature of 60 ℃, and filtering after decoloring to obtain a light yellow clear hydrolyzed keratin solution;
(5) purifying and concentrating the hydrolyzed keratin solution obtained in the step (4) by a membrane separation technology to obtain a yellow transparent keratin solution with the mass fraction of 18% and the molecular weight of 500 Da-2000 Da.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.

Claims (9)

1. A method for preparing a keratin solution by wool hydrolysis, which is characterized by comprising the following steps: the method for preparing the keratin solution by hydrolyzing the wool specifically comprises the following steps:
(1) soaking wool in an acid solution with a certain mass percentage concentration, heating for softening, cooling, washing with water, and drying to obtain acidified wool;
(2) adding the acidified wool obtained in the step (1) into water, dropwise adding alkali liquor under an ultrasonic condition to adjust the pH value to 8.0-10.5, and filtering;
(3) carrying out enzymolysis on the pretreated wool obtained in the step (2) by using subtilisin, inactivating enzyme after the enzymolysis is finished, adding activated carbon for decolorization, and filtering to obtain a hydrolyzed wool keratin dilute solution;
(4) and (4) concentrating the dilute hydrolyzed wool keratin solution obtained in the step (3) on a concentrating device to obtain a hydrolyzed keratin solution.
2. A method of wool hydrolysis for the preparation of a keratin solution as claimed in claim 1, characterized in that: the length of the wool in the step (1) is controlled below 5 cm.
3. A method for the preparation of a keratin solution by wool hydrolysis according to claim 1 or 2, characterized in that: the acid solution in the step (1) is one or more of acetic acid, oxalic acid, citric acid, hydrochloric acid, sulfuric acid or lactic acid, and the mass percentage concentration of the acid solution is 3-15%.
4. A method of wool hydrolysis for the preparation of a keratin solution as claimed in claim 3, characterized in that: in the step (1), wool and an acid solution are mixed according to a mass ratio of 1: feeding materials at a ratio of 5-1: 20, treating for 4-24 hours at a temperature of 60-90 ℃, and drying after cooling and water washing.
5. A method of wool hydrolysis for the preparation of a keratin solution as claimed in claim 1, characterized in that: the alkali liquor in the step (2) is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium sulfite or sodium bisulfite.
6. A method for the preparation of a keratin solution by wool hydrolysis according to claim 1 or 2, characterized in that: in the step (3), the mass percentage of the subtilisin in the acidified wool solution is 0.1-15%.
7. A method of wool hydrolysis for the preparation of a keratin solution as claimed in claim 6, characterized in that: the temperature of the enzymolysis step in the step (3) is 40-75 ℃, the enzymolysis PH = 8.0-10.5, the enzymolysis time is 16-72 h, and the enzyme deactivation condition is heat preservation treatment for 0.5-2 h at the temperature of 70-90 ℃; the mass ratio of the active carbon to the enzymolysis solution is (0.1-1): 100, the decoloring temperature is 60-90 ℃, and the decoloring time is 0.5-4 h.
8. A method for the preparation of a keratin solution by wool hydrolysis according to claim 1 or 2, characterized in that: the temperature of the enzymolysis step in the step (3) is 50 ℃, the enzymolysis PH =9, the enzymolysis time is 36h, and the enzyme deactivation condition is that the heat preservation treatment is carried out for 0.5h under the condition of 80 ℃; the mass ratio of the active carbon to the enzymolysis solution is 1:100, the decoloring temperature is 80 ℃, and the decoloring time is 1.5 h.
9. A method for the preparation of a keratin solution by wool hydrolysis according to claim 1 or 2, characterized in that: the hydrolyzed keratin solution in the step (4) is a clear and transparent yellow solution or a light yellow solution, the mass percentage is more than 18%, and the molecular weight is 500 Da-2000 Da.
CN202111352548.9A 2021-11-16 2021-11-16 Method for preparing keratin solution by wool hydrolysis Pending CN113855588A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111352548.9A CN113855588A (en) 2021-11-16 2021-11-16 Method for preparing keratin solution by wool hydrolysis

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111352548.9A CN113855588A (en) 2021-11-16 2021-11-16 Method for preparing keratin solution by wool hydrolysis

Publications (1)

Publication Number Publication Date
CN113855588A true CN113855588A (en) 2021-12-31

Family

ID=78984757

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111352548.9A Pending CN113855588A (en) 2021-11-16 2021-11-16 Method for preparing keratin solution by wool hydrolysis

Country Status (1)

Country Link
CN (1) CN113855588A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114456253A (en) * 2022-03-01 2022-05-10 上海天同纺织科技有限公司 Waste wool dissolving and keratin extracting process

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH037595A (en) * 1989-06-06 1991-01-14 Seiwa Kasei:Kk Production of keratin hydrolyzate
CN108727485A (en) * 2018-06-07 2018-11-02 河南双汇投资发展股份有限公司 A kind of preparation method of food-grade hydrolysis of keratin
CN108794614A (en) * 2018-06-21 2018-11-13 澳洋集团有限公司 The method for extracting wool keratin from waste wool

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH037595A (en) * 1989-06-06 1991-01-14 Seiwa Kasei:Kk Production of keratin hydrolyzate
CN108727485A (en) * 2018-06-07 2018-11-02 河南双汇投资发展股份有限公司 A kind of preparation method of food-grade hydrolysis of keratin
CN108794614A (en) * 2018-06-21 2018-11-13 澳洋集团有限公司 The method for extracting wool keratin from waste wool

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114456253A (en) * 2022-03-01 2022-05-10 上海天同纺织科技有限公司 Waste wool dissolving and keratin extracting process

Similar Documents

Publication Publication Date Title
CN103613652B (en) A kind of method of purification of silk fibroin
CN104789630B (en) A kind of bluefin tuna ossein hydrolysate and preparation method thereof
CN102492760A (en) Method for producing active Rana dybowskii collagen oligopeptide by using compound enzyme
CN109897101B (en) Collagen tripeptide and production method and application thereof
CN100369929C (en) Jellyfish collagen and method for preparing the same
CN113855588A (en) Method for preparing keratin solution by wool hydrolysis
KR20100092925A (en) Compositions for enhancing activity of cells, and face or skin filler comprising the polynucleotide fragments complex separated from fish's semen or egg
CN102732592A (en) Method for preparing freshwater fish bone gelatin by enzyme process
CN103829029A (en) Production method of non-denatured pure sericin stock solution
CN108148131A (en) The method that collagen is extracted from squid skin
CN110357978A (en) A kind of preparation method of selenide of carragheen
CN113563459A (en) Protein extraction process in production process of collagen peptide
CN1582771A (en) Production of collagen peptide from fish skins
CN103923963A (en) Method for preparing fish skin collagen and ACE inhibitory peptide
CN110100943A (en) A kind of raising immunity fish collagen protein powder and preparation method thereof
CN110257198B (en) Method for preparing facial soap from natural sericin stock solution
CN104513842A (en) Production method of odorless moisture-retaining collagen
CN108277247A (en) The method that antioxidant activity polypeptide is extracted from squid spawn tangled gland
US1602958A (en) Flavoring compound and method of making same
Wang et al. Design and experimental study on closed‐loop process of preparing chitosan from crab shells
CA1279329C (en) Process for the preparation of an aqueous solution of sodium methionine
CN111808903A (en) Safe and efficient novel protein antifreeze agent and preparation method and application thereof
JPH0790182A (en) Silk fibroin excellent in shelf stability and its production
CN111333554A (en) Method for preparing cystine by using hair
CN105602457B (en) A kind of method that gelatin is prepared by raw material of poultry skin and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20211231

RJ01 Rejection of invention patent application after publication