CN106905425A - A kind of preparation method of regenerated silk fibroin - Google Patents

A kind of preparation method of regenerated silk fibroin Download PDF

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Publication number
CN106905425A
CN106905425A CN201710248469.0A CN201710248469A CN106905425A CN 106905425 A CN106905425 A CN 106905425A CN 201710248469 A CN201710248469 A CN 201710248469A CN 106905425 A CN106905425 A CN 106905425A
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China
Prior art keywords
silk fibroin
regenerated silk
fibroin
salt
molten
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Pending
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CN201710248469.0A
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Chinese (zh)
Inventor
刘小玲
陈佳弘
赵谋明
江虹锐
余炼
王成华
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Guangxi University
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Guangxi University
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Priority to CN201710248469.0A priority Critical patent/CN106905425A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K14/00Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
    • C07K14/435Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
    • C07K14/43504Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
    • C07K14/43563Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects
    • C07K14/43586Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects from silkworms

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Zoology (AREA)
  • Biochemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Toxicology (AREA)
  • Tropical Medicine & Parasitology (AREA)
  • Biophysics (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Gastroenterology & Hepatology (AREA)
  • Molecular Biology (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Insects & Arthropods (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Cosmetics (AREA)
  • Peptides Or Proteins (AREA)

Abstract

The invention discloses a kind of preparation method of regenerated silk fibroin, specifically by through the discarded silk of thermokalite degumming including through salt is molten, coarse filtration, ultrafiltration, dry including step and obtain;It is that degumming fibroin albumen is put into mixing salt solution that wherein salt is molten, and 10~15min is heated at 85~100 DEG C;The mixing salt solution is the ethanol water of the calcium chloride of 3.5~4.5mol/L, and the ethanol volume accounting wherein in ethanol water is 20~40%.The inventive method prepares the scheme of regenerated silk fibroin compared with prior art, and the dissolved efficiency of fibroin albumen and acquired regenerated silk fibroin dissolubility, product yield reach splendid value simultaneously;The molecular weight distribution of resulting regenerated silk fibroin product is in 35~245kDa.The inventive method technique takes that short, efficiency high, effect are good, contributes to regenerated silk fibroin in the further genralrlization application in the fields such as food.

Description

A kind of preparation method of regenerated silk fibroin
Technical field
The present invention relates to the preparation of fibroin albumen, more particularly to a kind of preparation method of regenerated silk fibroin.
Background technology
Natural fibroin albumen has antiparallel beta sheet structure, in intermolecular and intramolecular hydrogen bond and Van der Waals force In the presence of Stability Analysis of Structures, it is therefore water insoluble.Insoluble natural fibroin albumen is changed into soluble regenerated silk fibroin (regenerated silk fibroin, RSF), can expand its application field;Regenerated silk fibroin and tissue biofacies Capacitive is high, and Medicated Permeation is strong, and good mechanical performance and degradability, can be applied to biomedicine, medical equipment, tissue Engineering and delivery system;In terms of food, research shows that regenerated silk fibroin has reducing blood lipid, promotes alcohol metabolism and drop The effects such as blood sugar, make an addition to and can have additional nutrients in food, promote health;Research also found that regenerated silk fibroin can also change The processing characteristics of kind food.A series of Japanese early beverage for having been developed that addition regenerated silk fibroins, fruit wine and cake, it is domestic Having researcher improves the mouthfeel of cake using the good foaming characteristic of regenerated silk fibroin.
Find that prior art is mainly to be studied the application of regenerated silk fibroin through retrieval, and to fibroin albumen Dissolving further investigate, the preparation process for regenerated silk fibroin does not carry out case study substantially, especially not to again The preparation method of raw silk fibroin is studied with the relation of yield, efficiency and properties of product.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the regenerated silk fibroin that dissolubility is good, production efficiency is high.
The preparation method of regenerated silk fibroin of the present invention, specifically by through the discarded silk of thermokalite degumming include through salt it is molten, Coarse filtration, ultrafiltration, drying are obtained in interior step;The salt is molten, is that the degumming fibroin albumen input that will be obtained through thermokalite degumming is mixed Salting liquid is closed, 10~15min is heated at 85~100 DEG C;The mixing salt solution is preferably using the chlorination of 3.5~4.5mol/L Ethanol volume accounting in the ethanol water of calcium, wherein ethanol water is 20~40%.The input amount of the mixing salt solution Can be selected according to general knowledge by one of ordinary skill in the art, it is molten preferably to put into 15ml~20ml salt-mixtures by every gram of degumming fibroin albumen Liquid.
In above method, preferred ultrafiltration, drying process are:The silk fibroin protein solution obtained after the molten step of salt is through thick After filter, using 5KDa ultrafiltration desalinations, then it is spray-dried.
The present invention have studied the condition that insoluble fibroin albumen changes to soluble regenerated silk fibroin, with fibroin albumen The dissolubility of production efficiency and regenerated silk fibroin is index analysis dissolution system, temperature, salinity and concentration of alcohol to silk The influence of fibroin dissolving, works out a kind of preparation technology of the regenerated silk fibroin that can be applied to food.Experiment shows:Pass through The preferred fibroin albumen molten technique of salt of the above, the inventive method prepares the scheme of regenerated silk fibroin compared with prior art, silk The parameter such as the dissolved efficiency of fibroin and acquired regenerated silk fibroin dissolubility, product yield reaches splendid value simultaneously;Institute The molecular weight distribution of the regenerated silk fibroin product for obtaining in 35~245kDa, suitably as the wall material raw material of microcapsule product. The inventive method technique takes that short, efficiency high, effect are good, contributes to regenerated silk fibroin in the further genralrlization in the fields such as food Using.
Specific embodiment
With reference to specific embodiment, comparative example and corresponding experimental data, further to regenerated silk fibroin of the present invention The concrete technical scheme and effect of preparation method are illustrated.It should be understood that these embodiments be only for explanation the present invention without For limiting embodiments of the present invention.
The embodiment of regenerated silk fibroin preparation method of the present invention:The preparation of regenerated silk fibroin of the present invention is first will be discarded Silk thermokalite degumming, then through including salt is molten, coarse filtration, ultrafiltration, the step including drying and obtain powdered regenerated silk fibroin Product;Wherein thermokalite degumming, coarse filtration, ultrafiltration, drying can refer to and use prior art, and salt is molten using following technique:Will be through heat The degumming fibroin albumen that alkali degumming is obtained, 15ml mixing salt solutions are put into by every gram of degumming fibroin albumen, are added at 85~100 DEG C 10~15min of heat;The mixing salt solution is the ethanol water of the calcium chloride of 3.5~4.5mol/L, wherein ethanol water In ethanol volume accounting be 20~40%.It is preferably super through 5KDa after the silk fibroin protein solution obtained after the molten step of salt is through coarse filtration Filter desalination, is then spray-dried, that is, obtain regenerated silk fibroin powdery product.Experiment is shown, is prepared using this technique Regenerated silk fibroin, fibroin albumen is completely dissolved time 3~13min of average out to, average regenerated silk fibroin yield up to 94%, Regenerated silk fibroin dissolubility (NSI) is 91~93%, and the average desalination time is 1.5~2.5 hours, shows the molten of fibroin albumen Solution efficiency is higher;Acquired regenerated silk fibroin dissolubility is good, regenerated silk fibroin molecular weight distribution in 35~245kDa, after Continuous experiment has preferably emulsifying capacity and emulsion stability when confirming to be used cooperatively with other raw materials, is suitably produced as microcapsules The wall material raw material of product.
Table 1 below -3 is respectively implementation comparative example and corresponding the experimental data (note that different process prepares regenerated silk fibroin: The difference of each embodiment is that the molten step of salt employs different technological parameters in table, and other steps are using institute above State, identical technique):
Table 1
Table 2
Table 3
Above experimental data shows, by the preferred molten technique of fibroin albumen salt, using the inventive method preparation regenerated silk During fibroin, the dissolved efficiency of fibroin albumen and acquired regenerated silk fibroin dissolubility, regenerated silk fibroin yield are simultaneously Splendid value is reached, and the desalination time is shorter.
Above content is only some better embodiments enumerated to introduce technical solution of the present invention, be not construed as Limit form of implementation of the invention.The equivalent variations that all one of ordinary skill in the art can make according to technical solution of the present invention with change Enter, all should belong within the covering scope of technical solution of the present invention.

Claims (3)

1. a kind of preparation method of regenerated silk fibroin, it is characterised in that:It is that will include through salt through the discarded silk of thermokalite degumming Molten, coarse filtration, ultrafiltration, drying are obtained in interior step;
The salt is molten, is the degumming fibroin albumen input mixing salt solution that will be obtained through thermokalite degumming, is heated at 85~100 DEG C 10~15min;The mixing salt solution is the ethanol water of the calcium chloride of 3.5~4.5mol/L, wherein in ethanol water Ethanol volume accounting be 20~40%.
2. the preparation method of regenerated silk fibroin according to claim 1, it is characterised in that:Obtained after the molten step of salt Silk fibroin protein solution through coarse filtration after, using 5KDa ultrafiltration desalinations, be then spray-dried.
3. the preparation method of regenerated silk fibroin according to claim 1 and 2, it is characterised in that institute in the molten step of salt The usage amount for stating mixing salt solution is:Every gram of degumming fibroin albumen puts into 15~20ml mixing salt solutions.
CN201710248469.0A 2017-04-14 2017-04-14 A kind of preparation method of regenerated silk fibroin Pending CN106905425A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102775465A (en) * 2012-08-01 2012-11-14 中国人民解放军第三军医大学 Method for preparing regenerative silk fibroin and product and application thereof
CN103768654A (en) * 2012-10-18 2014-05-07 上海纳米技术及应用国家工程研究中心有限公司 Water-soluble fibroin powder and preparation method thereof
CN105534869A (en) * 2016-01-30 2016-05-04 常州市鼎升环保科技有限公司 Preparation method for anti-ultraviolet silk fibroin
CN106046135A (en) * 2016-08-08 2016-10-26 南通大学 Silk fibroins with different degradation rates and use thereof
CN106243210A (en) * 2016-08-12 2016-12-21 西南大学 A kind of less salt anhydrous solvent system dissolves the method for natural silk

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102775465A (en) * 2012-08-01 2012-11-14 中国人民解放军第三军医大学 Method for preparing regenerative silk fibroin and product and application thereof
CN103768654A (en) * 2012-10-18 2014-05-07 上海纳米技术及应用国家工程研究中心有限公司 Water-soluble fibroin powder and preparation method thereof
CN105534869A (en) * 2016-01-30 2016-05-04 常州市鼎升环保科技有限公司 Preparation method for anti-ultraviolet silk fibroin
CN106046135A (en) * 2016-08-08 2016-10-26 南通大学 Silk fibroins with different degradation rates and use thereof
CN106243210A (en) * 2016-08-12 2016-12-21 西南大学 A kind of less salt anhydrous solvent system dissolves the method for natural silk

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘晨: "离心纺不同分子量再生丝素蛋白的可纺性研究", 《中国优秀硕士学位论文全文数据库》 *
苏州丝绸工学院: "《高等纺织院校教材 制丝化学》", 31 October 1979 *

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Application publication date: 20170630