CN1101402C - Sericin polypeptide extracted from frison, husks and waste silk and its extracting method - Google Patents

Sericin polypeptide extracted from frison, husks and waste silk and its extracting method Download PDF

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Publication number
CN1101402C
CN1101402C CN98123202A CN98123202A CN1101402C CN 1101402 C CN1101402 C CN 1101402C CN 98123202 A CN98123202 A CN 98123202A CN 98123202 A CN98123202 A CN 98123202A CN 1101402 C CN1101402 C CN 1101402C
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China
Prior art keywords
sericin polypeptide
sericin
solution
sericine
raw material
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CN98123202A
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CN1228438A (en
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陈文兴
刘冠峰
隋秀芝
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ZHEJIANG SILK ENGINEERING INST
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ZHEJIANG SILK ENGINEERING INST
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  • Enzymes And Modification Thereof (AREA)
  • Cosmetics (AREA)

Abstract

The present invention relates to sericin polypeptide extracted from cocoon frison, cocoon shells and waste silk, which is sericin polypeptide directly extracted from cocoon frison, cocoon shells and waste silk and prepared by using an enzymatic hydrolysis technology. The average molecular weight of the sericin polypeptide is from 200 to 5000. The forms of products can be solution or powder, and the prepared sericin polypeptide can be used as the raw materials of cosmetics. The sericin polypeptide contains 20.3 mol% of essential amino acids necessary for human bodies and 75.1 mol% of polar amino acids. Therefore, the sericin polypeptide has the advantages of good hygroscopicity, temperature preserving performance and nutritive value. The extraction method has the advantages of high simplicity and practicality and low cost, precious natural protein resources are utilized, and environment is protected.

Description

Sericin polypeptide and the method from husks, cocoon shell, waste silk, extracted
The present invention relates to a kind of daily cosmetics raw material and extracting method thereof.
The silk fiber is made up of 20~30% sericine and 70~80% fibroin protein, and sericine content is more up to 40% in husks.Wherein fibroin protein not only is made into silk, but also is developed to the raw material of makeup and food.Relative therewith, sericine is not but by practical application, and this has not only wasted valuable natural protein resource, but also has polluted environment.Its reason mainly is to extract and prepare the technology more complicated of sericin polypeptide, cost height from filature, refining wastewater.
In view of the foregoing, the purpose of this invention is to provide a kind of sericine that directly extracts from husks, cocoon shell, waste silk is hydrolyzed into easily by the sericin polypeptide and the extracting method of skin and hair absorption.
The present invention is in direct any raw material from husks, cocoon shell, waste silk, adds water and proteolysis enzyme extraction sericin polypeptide.
A kind of method of directly from husks, cocoon shell, waste silk, extracting sericin polypeptide that is exclusively used in:
1. add water in raw material, the bath raio of raw material and water is 1: 10~200;
2. be heated to 80~150 ℃ of sericines in the dissolving raw material;
3. the taking-up fibroin gets sericine solution;
4. carry out or do not carry out concentration;
5. attemperation and pH value are to the suitable hydrolysising condition of used proteolytic ferment;
6. add proteolytic ferment and impel the sericine hydrolysis, the consumption of enzyme is the sericine solid weight
0.01~20%, hydrolysis time is 5 minutes~24 hours;
7. solution being added the heat kill enzyme handles;
8. remove by filter insolubles, get shallow tawny sericin polypeptide solution.
Another kind is exclusively used in the method for directly extracting sericin polypeptide from husks, cocoon shell, waste silk:
1. the water that adds room temperature~100 ℃ in raw material carries out pre-soaking, and the bath raio of raw material and water is 1: 10~200;
2. attemperation and pH value are to the optimum hydrolysising condition of used proteolytic ferment;
3. add proteolytic ferment and impel sericine hydrolysis and dissolving, the consumption of enzyme is the sericine solid
0.01~20% of weight, hydrolysis and dissolution time are 5 minutes~24 hours;
4. taking-up fibroin;
5. solution being added the heat kill enzyme handles;
6. remove by filter insolubles, get shallow tawny sericin polypeptide solution.
Sericin polypeptide solution is decoloured or/and concentration.In sericin polypeptide solution, add sanitas and tensio-active agent again, or be dried to the sericin polypeptide powder.
The present invention is the sericin polypeptide of the direct sericine that extracts from husks, cocoon shell, waste silk through hydrolysis, and it is motivated, and method is simple, and is economical and practical, and cost is low, is to the utilization of the natural protein resource of preciousness, also helps the protection of environment.Owing to contain the essential amino acid of 20.3mol% and the polare Aminosaeren of 75.1mol% in the sericin polypeptide, thereby have good water absorbability, moisture retention and nutritive value.
When extracting sericine solution with hot water from husks, cocoon shell, waste silk, its solvent temperature is more than 80 ℃, and dissolution time is decided according to temperature, and the high time of temperature is short, and the low time of temperature is long, dissolves the economic again purpose of sericine to reach as far as possible.Proteolytic enzyme comprise can the hydrolysis sericine various enzymes, as trypsinase, stomach en-, papoid, bacteria protease.The temperature of enzymolysis and pH value are determined according to the optimum hydrolysising condition of each enzyme.The add-on of enzyme is generally 0.01~20% of sericine solid weight.Enzymolysis time is determined according to the stability of sericin polypeptide solution and the molecular weight of required sericin polypeptide.During as cosmetic material, the control molecular-weight average is advisable between 200~5000, and the sericin polypeptide solution of this molecular weight ranges is generally comparatively stable.In the sericin polypeptide that extracts, add sanitas and tensio-active agent or be dried to of the preservation of sericin polypeptide powder in order to product.
The amino acid of sericine and fibroin protein is formed as shown in table 1, as known from Table 1, the essential amino acid in the sericine and the content of polare Aminosaeren are far above the content of essential amino acid in the fibroin protein and polare Aminosaeren, so sericin polypeptide has better water absorbability, moisture retention and nutritive value than fibroin polypeptide.
Sericin polypeptide has significant protection and trophism to people's hair and skin.After the Hair grooming sericin polypeptide solution impregnation, elasticity and flexibility increase, and glossiness is good, the damage that can repair and protect hair to be subjected to.After skin applied with sericin polypeptide solution, water absorbability and moisture retention obviously increased, and can suppress dermal melanin formation, impelled skin tissue regeneration.
The amino acid of table 1 sericine and fibroin protein is formed (mol%)
The amino acid title Sericine Fibroin protein
Essential amino acid Threonine 8.3 0.9
Methionin 4.3 0.3
Arginine 2.8 0.5
Xie Ansuan 3.1 2.2
Leucine 0.8 0.5
Isoleucine 0.6 0.7
Tryptophane 0.3 0.2
Methionine(Met) 0.1 0.1
Serine 33.1 12.1
Halfcystine 0.3 0.2
Aspartic acid 14.6 1.3
L-glutamic acid 7.9 1.0
Glycocoll 13.5 44.5
L-Ala 5.2 29.3
Histidine 1.0 0.2
Phenylalanine 0.5 0.6
Tyrosine 3.1 5.2
Proline(Pro) 0.5 0.3
Add up to Essential amino acid 20.3 5.4
Polare Aminosaeren (Ap) 75.1 21.5
Nonpolar amino acid (An) 24.9 78.6
Ap/An 3.02 0.27
Below be concrete embodiment, but not as limit.
Embodiment 1 (method 2)
Get cocoon shell 5Kg, add water 200Kg, 90 ℃ were soaked 1 hour, regulate pH value to 9 with NaOH solution when being cooled to 45 ℃, behind the adding 3g bacteria protease, be incubated 2 hours, make sericine hydrolysis and dissolving, take out fibroin, be warmed to 90 ℃ of insulations again and killed the enzyme processing in 10 minutes.Solution removes by filter insolubles, gets shallow dark brown sericin polypeptide dilute solution.With the gac processing of decolouring, by concentrate, lyophilize gets the powdery sericin polypeptide, its molecular-weight average is about 2500.
Embodiment 2 (method 2)
Get husks 5Kg, removal of impurities adds water 150Kg after cleaning, and is heated to 40 ℃, regulates pH value to 8.5 with NaOH, adds 6g trypsinase insulation 3 hours, makes sericine hydrolysis and dissolving, takes out fibroin, and reheat to 85 a ℃ insulation was killed enzyme in 15 minutes and handled.Solution removes by filter insolubles, gets shallow dark brown sericin polypeptide solution, and its molecular-weight average is about 2000, after concentrating, adds sanitas, tensio-active agent.
Embodiment 3 (method 1)
Get husks 6Kg, after removal of impurities is cleaned, add water 200Kg, being warmed to 100 ℃ boiled 2 hours, make the sericine dissolving, fibroin is taken out in cooling, gets sericine solution, regulate pH value to 9 with NaOH solution, add the 5g bacteria protease, 40 ℃ are incubated 2 hours, make the sericine hydrolysis, reheat to 80 a ℃ maintenance was killed enzyme in 15 minutes and is handled, the elimination insolubles, shallow dark brown sericin polypeptide dilute solution, by concentrate sericin polypeptide solution, its molecular-weight average is about 1500, adds sanitas, tensio-active agent.
Embodiment 4 (method 1)
Get waste silk 8Kg, clean and add water 240Kg, be heated to 120 ℃ of insulations 1 hour, make the sericine dissolving, fibroin is taken out in cooling, sericine solution, concentrate and to make 3% sericine solution, be heated to 70 ℃ and regulate pH value to 5 with HCl solution, add the 4g papoid, be incubated 1 hour, reheat to 100 a ℃ insulation was killed enzyme in 10 minutes and is handled, and solution removes by filter insolubles, get shallow tawny sericin polypeptide solution, its molecular-weight average is about 3000, handles with activated carbon decolorizing, adds sanitas, tensio-active agent again.

Claims (5)

1. the sericin polypeptide that extracts from husks, cocoon shell, waste silk is characterized in that: the sericin polypeptide of water and proteolysis enzyme extraction in direct any raw material in husks, cocoon shell, waste silk.
2. one kind is exclusively used in the method for extracting the described sericin polypeptide of claim 1:
1) add water in raw material, the bath raio of raw material and water is 1: 10~200;
2) be heated to 80~150 ℃ of sericines in the dissolving raw material;
3) take out fibroin, get sericine solution;
4) carry out or do not carry out concentration;
5) attemperation and pH value are to the suitable hydrolysising condition of used proteolytic ferment;
6) add proteolytic ferment and impel the sericine hydrolysis, the consumption of enzyme is the sericine solid weight
0.01~20%, hydrolysis time is 5 minutes~24 hours;
7) solution being added the heat kill enzyme handles;
8) remove by filter insolubles, get shallow tawny sericin polypeptide solution.
3. the another kind of method of extracting the described sericin polypeptide of claim 1 that is exclusively used in:
1) water that adds room temperature~100 ℃ in raw material carries out pre-soaking, and the bath raio of raw material and water is 1: 10~200;
2) attemperation and pH value are to the suitable hydrolysising condition of used proteolytic ferment;
3) add proteolytic ferment and impel sericine hydrolysis and dissolving, the consumption of enzyme is the sericine solid
0.01~20% of weight, hydrolysis and dissolution time are 5 minutes~24 hours;
4) take out fibroin;
5) solution being added the heat kill enzyme handles;
6) remove by filter insolubles, get shallow tawny sericin polypeptide solution.
4. according to claim 2 or 3 described methods, it is characterized in that: sericin polypeptide solution is decoloured or/and concentration.
5. according to claim 2 or 3 described methods, it is characterized in that: in sericin polypeptide solution, add sanitas and tensio-active agent again, or be dried to the sericin polypeptide powder.
CN98123202A 1998-12-01 1998-12-01 Sericin polypeptide extracted from frison, husks and waste silk and its extracting method Expired - Fee Related CN1101402C (en)

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CN1101402C true CN1101402C (en) 2003-02-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250995A (en) * 2011-03-25 2011-11-23 兴化市大地蓝绢纺有限公司 Method for degumming from silk spinning raw material and recovering sericin

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CN100999545B (en) * 2007-01-12 2010-09-08 东华大学 Process of recovering sericine by ion exchanging
CN101348821B (en) * 2008-08-29 2011-08-31 湖州南方生物科技有限公司 High purity sericin powder prepared from silkworm cocoon blaze and preparation thereof
CN102584430B (en) * 2012-01-10 2013-07-24 广西工学院 Method for manufacturing amino-acid fishpond fertilizer water aqua by waste bave protein
CN102618610B (en) * 2012-03-26 2013-12-04 苏州大学 Preparation method of sericin compound amino acid
CN102961298A (en) * 2012-12-21 2013-03-13 李卫旗 Manufacturing method of body lotion by taking Pullulan polysaccharide and sericin bioactive peptide as main raw materials
CN103006518A (en) * 2013-01-07 2013-04-03 李卫旗 Method for preparing novel nutrient recovery type skin-care facial mask
CN103301033B (en) * 2013-05-30 2015-03-25 南通缘生堂生物科技有限公司 Preparation method of ultramicro silk fibroin powder
CN105017386A (en) * 2015-07-28 2015-11-04 苏州普罗达生物科技有限公司 Sericin polypeptide 2, and preparation and application thereof
CN105326760A (en) * 2015-11-30 2016-02-17 河池学院 Soaking-free silkworm cocoon composition, preparation method and application of soaking-free silkworm cocoon composition in skin whitening
CN106512080A (en) * 2016-11-24 2017-03-22 江苏爱西施科技服务咨询股份有限公司 Preparation method for sericin protein hydrogel
CN108041115A (en) * 2017-12-19 2018-05-18 牟小林 A kind of food compounding moisturizer containing silk gum and preparation method thereof
CN110499350B (en) * 2019-03-15 2021-02-02 辽东学院 Sericin hydrolysis method, product and application thereof
CN114404568B (en) * 2022-01-16 2023-12-26 重庆理工大学 Sericin polypeptide injection preparation and application thereof

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CN1050197A (en) * 1990-10-31 1991-03-27 上海丝织地毯厂 Extract the method for silk-protein from carpet leftover bits and pieces waste silk
CN1128764A (en) * 1995-05-24 1996-08-14 复旦大学 Regenerated silk protein and complex material thereof for fixation of enzyme and bio-active substance
CN1150438A (en) * 1995-01-27 1997-05-21 农林水产省蚕丝昆虫农业技术研究所长 Process for producing fine silk fibroin powder
CN1191863A (en) * 1997-02-25 1998-09-02 浙江省商业集团进出口公司 Chitin preparing process using crust of silkworm chrysalis

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1050197A (en) * 1990-10-31 1991-03-27 上海丝织地毯厂 Extract the method for silk-protein from carpet leftover bits and pieces waste silk
CN1150438A (en) * 1995-01-27 1997-05-21 农林水产省蚕丝昆虫农业技术研究所长 Process for producing fine silk fibroin powder
CN1128764A (en) * 1995-05-24 1996-08-14 复旦大学 Regenerated silk protein and complex material thereof for fixation of enzyme and bio-active substance
CN1191863A (en) * 1997-02-25 1998-09-02 浙江省商业集团进出口公司 Chitin preparing process using crust of silkworm chrysalis

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102250995A (en) * 2011-03-25 2011-11-23 兴化市大地蓝绢纺有限公司 Method for degumming from silk spinning raw material and recovering sericin
CN102250995B (en) * 2011-03-25 2012-07-04 兴化市大地蓝绢纺有限公司 Method for degumming from silk spinning raw material and recovering sericin

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