CN101974596A - Extraction method of silk peptide - Google Patents

Extraction method of silk peptide Download PDF

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Publication number
CN101974596A
CN101974596A CN 201010540602 CN201010540602A CN101974596A CN 101974596 A CN101974596 A CN 101974596A CN 201010540602 CN201010540602 CN 201010540602 CN 201010540602 A CN201010540602 A CN 201010540602A CN 101974596 A CN101974596 A CN 101974596A
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China
Prior art keywords
silk
enzymolysis
useless
peptide
silk peptide
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CN 201010540602
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叶传发
张小东
胡承四
叶思
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HUBEI YUANCHENG PHARMACEUTICAL CO Ltd
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HUBEI YUANCHENG PHARMACEUTICAL CO Ltd
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Priority to CN 201010540602 priority Critical patent/CN101974596A/en
Publication of CN101974596A publication Critical patent/CN101974596A/en
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Abstract

The invention discloses an extraction method of a silk peptide, comprising the following steps of: edulcorating waste silk as a main raw material; blending the waste silk with water; adding sodium sulfite for warming and stewing; filtering; carrying out protease enzymolysis; inactivating enzymes; decoloring; separating a membrane; and drying obtained filter liquor to obtain the silk peptide. The extraction method has short production period and low cost without generating any toxic and harmful substance; and in addition, the obtained product has high safety and can be widely used in the fields of cosmetics, foods, drugs, and the like.

Description

A kind of extracting method of silk peptide
Technical field
The inventive method relates to useless silk, silk cocoon deep process technology field, is specifically related to a kind of extracting method of silk peptide, be a kind of be raw material with useless silk, utilize the biological enzyme enzymolysis silk that give up, thus the method for extraction silk peptide.
Background technology
Useless silk is the tankage in the silk course of processing, with producing molecular weight behind the special protease hydrolyzed below 1000 dalton but active very high small peptide molecule.Silk peptide is absorbed by hair easily and is difficult for being gone by washing, and silk peptide is very similar to the Keratin sulfate in the hair, and hair is had higher affinity, and the permeable hair that enters plays nutrition and the effect of repairing damage to lamina corticalis.Being rich in the amino acid of needed by human in the silk peptide, is again a kind of pure protein, it can control blood sugar for human body amount, have reducing cholesterol and promote the effect that alcohol decomposes, autoimmune disorder is had good preventive and therapeutic effect.
Extracting silk peptide from useless silk at home and abroad all is a kind of industry in the ascendant, but majority all is to finish by following steps: useless silk → alkaline purification → high temperature steaming → enzymolysis → filtration → concentrate → spraying drying, with a large amount of alkaline purifications, both bring serious environmental to pollute and potential safety hazard, destroyed proteinic composition again; And concentrate the product phase of destroying product easily, and do not use membrane separation technique in the prior art, influenced the quality of product.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of extracting method of silk peptide is provided, be a kind ofly to need not to use alkaline purification, and utilize the biological enzyme enzymolysis, with the membrane separation technique desalination with concentrate the method that obtains the finished product.
In order to achieve the above object, the present invention adopts following technical measures:
A kind of extracting method of silk peptide, its step is as follows:
1) the useless silk removal of impurities of raw material;
2) by 7 water extraordinarily of useless silk weight, add S-WAT by 1% of useless silk weight again and stir 100 ℃ of boiling 4-6h;
3) boiling finishes, and is cooled to 51-55 ℃, and adjust pH is 8.0-8.5, adds Sumizyme MP by 1% of useless silk weight, and constant temperature stirs enzymolysis 4-6h;
4) enzymolysis solution that obtains is warming up to 92-95 ℃, the constant temperature enzyme 10-14min that goes out;
5) enzymolysis solution is filtered, get supernatant liquor;
6) 2-2.5% by useless silk weight adds powdered active carbon in the supernatant liquor, and 45-50 ℃ is stirred 1-1.5h, remove by filter gac;
7) filtered liquid is used membrane separation technique desalination and concentrated;
8) concentrated solution is spray-dried, obtain the product silk peptide.
The vigor of the Sumizyme MP that uses in the inventive method is 2.5 ten thousand U/g.
Compared with prior art, advantage of the inventive method and beneficial effect are as follows:
1, effectively avoided the environmental pollution that alkaline purification in the prior art brought, and the racemization that causes of alkali is to the reduction of product nutritive value;
2, the silk peptide produced of the inventive method, the content of the peptide of molecular weight below 1000 dalton reaches more than 95% in its gross protein, and wherein the content of Serine reaches more than 35%;
3, the membrane separation technique in the inventive method, but the liquid towards material separates, concentrate and purifying, and all operate at normal temperatures, do not have phase-state change, energy-efficient, do not produce pollution in the production process;
4, the inventive method is with short production cycle, cost is low, do not produce any hazardous and noxious substances, and safety has no side effect, and can be widely used in fields such as makeup, food, medicine.
Embodiment
Below in conjunction with specific embodiment the inventive method is described in further detail.
Embodiment 1:
A kind of extracting method of silk peptide, step is as follows:
(1kg of foreign matter content<15wt%) cleans and joins pure water 7kg after removing impurity, adds sodium sulphite anhydrous 99.3 10g again, stirs, and is warming up to 100 ℃ of boiling 4h to take by weighing useless silk; Be cooled to 51 ℃ again, transfer pH to 8.0 with the food grade flaky sodium hydrate, add the 10g Sumizyme MP, 51 ℃ of constant temperature stir enzymolysis 6h, reduce as the pH value in the enzymolysis process, regulate with food grade sodium hydroxide, keep stable; Be warming up to 95 ℃ then, the insulation 10min enzyme that goes out; Enzymolysis solution is filtered, get supernatant liquor; Add the 20g powdered active carbon in the supernatant liquor, 50 ℃ of whip attachment 1h decolourings, filtering gacs then; Filtrate is the collecting and filtering apparatus filtration of 1nm with membrane pore size, and desalination also concentrates; Concentrated solution is spray-dried, obtains the Powdered silk peptide of 400g white (the present invention has adopted gac to decolour, and the color and luster of products obtained therefrom is a white, is better than the faint yellow of national Specification), and the examining report of products obtained therefrom sees Table 1.
The examining report of table 1 embodiment 1 products obtained therefrom
Figure BDA0000031814600000031
Embodiment 2:
A kind of extracting method of silk peptide, step is as follows:
(2kg of foreign matter content<15wt%) cleans and joins pure water 14kg after removing impurity, adds sodium sulphite anhydrous 99.3 20g again, stirs, and is warming up to 100 ℃ of boiling 5h to take by weighing useless silk; Be cooled to 55 ℃ again, transfer pH to 8.1 with the food grade flaky sodium hydrate, add the 20g Sumizyme MP, 55 ℃ of constant temperature stir enzymolysis 5.5h, and pH value as reduction are regulated with food grade sodium hydroxide in the enzymolysis process, keep stable; Be warming up to 94 ℃ then, the insulation 12min enzyme that goes out; Enzymolysis solution is filtered, get supernatant liquor; Add the 40g powdered active carbon in the supernatant liquor, 48 ℃ of whip attachment 1.2h decolourings, filtering gacs then; Filtrate is the collecting and filtering apparatus filtration of 1nm with membrane pore size, and desalination also concentrates; Concentrated solution is spray-dried, obtains 800g white powder silk peptide, and the examining report of products obtained therefrom sees Table 2.
The examining report of table 2 embodiment 2 products obtained therefroms
Figure BDA0000031814600000032
Figure BDA0000031814600000041
Embodiment 3:
A kind of extracting method of silk peptide, step is as follows:
(10kg of foreign matter content<15wt%) cleans and joins pure water 70kg after removing impurity, adds sodium sulphite anhydrous 99.3 100g again, stirs, and is warming up to 100 ℃ of boiling 6h to take by weighing useless silk; Be cooled to 53 ℃ again, transfer pH to 8.2 with the food grade flaky sodium hydrate, add the 100g Sumizyme MP, 53 ℃ of constant temperature stir enzymolysis 5h, and pH value as reduction are regulated with food grade sodium hydroxide in the enzymolysis process, keep stable; Be warming up to 95 ℃ then, the insulation 11min enzyme that goes out; Enzymolysis solution is filtered, get supernatant liquor; Add the 200g powdered active carbon in the supernatant liquor, 47 ℃ of whip attachment 1.3h decolourings, filtering gacs then; Filtrate is the collecting and filtering apparatus filtration of 1nm with membrane pore size, and desalination also concentrates; Concentrated solution is spray-dried, obtains 4kg white powder silk peptide, and the examining report of products obtained therefrom sees Table 3.
The examining report of table 3 embodiment 3 products obtained therefroms
Figure BDA0000031814600000042
Embodiment 4:
A kind of extracting method of silk peptide, step is as follows:
(100kg of foreign matter content<15wt%) cleans and joins pure water 700kg after removing impurity, adds sodium sulphite anhydrous 99.3 1kg again, stirs, and is warming up to 100 ℃ of boiling 5.5h to take by weighing useless silk; Be cooled to 54 ℃ again, transfer pH to 8.5 with the food grade flaky sodium hydrate, add the 1kg Sumizyme MP, 54 ℃ of constant temperature stir enzymolysis 4h, and pH value as reduction are regulated with food grade sodium hydroxide in the enzymolysis process, keep stable; Be warming up to 92 ℃ then, the insulation 14min enzyme that goes out; Enzymolysis solution is filtered, get supernatant liquor; Add the 2.5kg powdered active carbon in the supernatant liquor, 45 ℃ of whip attachment 1.5h decolourings, filtering gacs then; Filtrate is the collecting and filtering apparatus filtration of 1nm with membrane pore size, and desalination also concentrates; Concentrated solution is spray-dried, obtains 40kg white powder silk peptide, and the examining report of products obtained therefrom sees Table 4.
The examining report of table 4 embodiment 4 products obtained therefroms
Figure BDA0000031814600000051

Claims (3)

1. the extracting method of a silk peptide, its step is as follows:
1), the useless silk removal of impurities of raw material;
2), by 7 water extraordinarily of useless silk weight, add S-WAT by 1% of useless silk weight again and stir 100 ℃ of boiling 4-6h;
3), boiling finishes, and is cooled to 51-55 ℃, adjust pH is 8.0-8.5, adds the Sumizyme MP of 2.5 ten thousand U/g by 1% of useless silk weight, constant temperature stirs enzymolysis 4-6h, keeps system pH stable with sodium hydroxide in the enzymolysis process;
4), the enzymolysis solution that obtains is warming up to 92-95 ℃, the constant temperature enzyme 10-14min that goes out;
5), enzymolysis solution is filtered, supernatant liquor;
6), the 2-2.5% by useless silk weight in the supernatant liquor adds powdered active carbon, 45-50 ℃ is stirred 1-1.5h, removes by filter gac;
7), filtered liquid is used membrane separation technique desalination and concentrated;
8), after the concentrated solution drying, obtain the product silk peptide.
2. the method for claim 1, it is characterized in that: the aperture of described film is 1nm.
3. the method for claim 1, it is characterized in that: described drying is a spraying drying.
CN 201010540602 2010-11-11 2010-11-11 Extraction method of silk peptide Pending CN101974596A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102206695A (en) * 2011-04-02 2011-10-05 重庆海帆生化科技有限公司 Method for preparing silk short peptides and silk amino acids by using waste silks
CN104761616A (en) * 2015-04-15 2015-07-08 海安县南莫制丝有限公司 Method for preparing soluble silk protein liquid employing waste silk
CN105982831A (en) * 2015-02-09 2016-10-05 郭宗卫 Cosmetic containing active peptide
CN107956126A (en) * 2017-11-27 2018-04-24 无锡昊瑜节能环保设备有限公司 A kind of real silk fabric anti-crease finishing technique
CN108424440A (en) * 2018-05-04 2018-08-21 杨恒智 Fibroin albumen, preparation method and its application in cosmetic skin, soft fabric arrange
CN109627309A (en) * 2018-12-28 2019-04-16 浙江工业大学 A method of silk peptide is prepared using serrapeptase hydrolysis fibroin
CN111205609A (en) * 2020-03-14 2020-05-29 浙江世博新材料股份有限公司 Novel PBT and preparation method thereof
CN112409469A (en) * 2020-11-04 2021-02-26 付俊 Extraction method of silk peptide
CN114957427A (en) * 2022-06-07 2022-08-30 浙江明亮生物科技有限责任公司 Method for preparing silk fibroin peptide by protease enzymolysis

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006014033A1 (en) * 2004-07-31 2006-02-09 Brainguard Co., Ltd. Silk peptide improving neuroprotective and neurofunctional effects and a method of its preparation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006014033A1 (en) * 2004-07-31 2006-02-09 Brainguard Co., Ltd. Silk peptide improving neuroprotective and neurofunctional effects and a method of its preparation

Non-Patent Citations (1)

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Title
《食品工业科技》 20100831 高光 牟光庆 碱性蛋白酶水解柞蚕丝素蛋白工艺的研究 1-3 第31卷, 第8期 2 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102206695A (en) * 2011-04-02 2011-10-05 重庆海帆生化科技有限公司 Method for preparing silk short peptides and silk amino acids by using waste silks
CN105982831A (en) * 2015-02-09 2016-10-05 郭宗卫 Cosmetic containing active peptide
CN104761616A (en) * 2015-04-15 2015-07-08 海安县南莫制丝有限公司 Method for preparing soluble silk protein liquid employing waste silk
CN107956126A (en) * 2017-11-27 2018-04-24 无锡昊瑜节能环保设备有限公司 A kind of real silk fabric anti-crease finishing technique
CN108424440A (en) * 2018-05-04 2018-08-21 杨恒智 Fibroin albumen, preparation method and its application in cosmetic skin, soft fabric arrange
CN109627309A (en) * 2018-12-28 2019-04-16 浙江工业大学 A method of silk peptide is prepared using serrapeptase hydrolysis fibroin
CN111205609A (en) * 2020-03-14 2020-05-29 浙江世博新材料股份有限公司 Novel PBT and preparation method thereof
CN112409469A (en) * 2020-11-04 2021-02-26 付俊 Extraction method of silk peptide
CN112409469B (en) * 2020-11-04 2023-09-26 付俊 Extraction method of silk peptide
CN114957427A (en) * 2022-06-07 2022-08-30 浙江明亮生物科技有限责任公司 Method for preparing silk fibroin peptide by protease enzymolysis

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Application publication date: 20110216