CN102417599B - Method for dissolving fibroin - Google Patents

Method for dissolving fibroin Download PDF

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Publication number
CN102417599B
CN102417599B CN 201010294430 CN201010294430A CN102417599B CN 102417599 B CN102417599 B CN 102417599B CN 201010294430 CN201010294430 CN 201010294430 CN 201010294430 A CN201010294430 A CN 201010294430A CN 102417599 B CN102417599 B CN 102417599B
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silk
protein
fibroin
room temperature
urea
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CN102417599A (en
Inventor
杨明英
朱良均
闵思佳
张海萍
杨磊
邓连霞
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a method for dissolving fibroin. The method comprises steps of: placing 3-10 g of fibroin into 40-60 ml of 6M-8M urea and adding 2.5-5 g of sodium hydroxide solid powder; or first dissolving 2.5-5 g of sodium hydroxide solid powder in 40-60 ml of 6M-8M urea and placing 3-10 g of fibroin into the solution; standing at room temperature for 4-24 hr; stirring uniformly under room temperature to obtain the fibroin solution. The invention has advantages of low energy consumption, high biological safety, low price, easy and convenient operation and no environmental pollution. In addition, waste liquid is easy for recovery and recycling; the fibroin powder prepared by the invention can be used as a raw material in fields of foodstuff, cosmetic, medicine and biomaterial, etc.

Description

A kind of method of dissolving silk-protein
Technical field
The present invention relates to the natural polymer field, particularly a kind of method of dissolving silk-protein.
Background technology
By Juvenile Hormone, wild silk yarn albumen (tussah silk and wild silk yarn etc.) and spider silk are protein fibres, because of its unique mechanical property and good biocompatibility, degradation property and stability, and essence is the constructional feature of protein, can obtain after treatment regenerated silk protein fiber, silk fibroin powder, fibroin protein film, fibroin porous material, be applied to the fields such as food, makeup, medicine, biomaterial.Natural silk albumen is synthetic in insect body, secretion, and the form with the silk protein aqueous solution of high density (30%) is stored in sericterium, in becoming the silk process, under the impact of process spinneret stretching and concentration of metal ions, pH value, form the wire protein fiber of satisfactory mechanical property.Yet, in case after forming silky fibre, wire protein fiber is difficult to be dissolved in water, can only be dissolved in concentrated hydrochloric acid, sulfuric acid, HFA, HFIP, formic acid, LiBr, LiSCN and CaCl 2Solution, and these harmful poisonous polar solvents are against in biological safety, cost is high and pollution arranged.China produces a silk big country, and sufficient waste cocoon and waste silk resource are arranged, and how to utilize at low cost the reclaiming of inferior horn cocoon, waste silk and spun silk fabric product resource, and one of gordian technique is exactly to find that cost is low, operational safety is simple and easy, environment amenable solvent.Japan Report (Japan PatentWO2009119596-A1) is placed in the 8M urea soln to By Juvenile Hormone and heats to 200 ℃, can dissolve silk-protein, but the conditions such as solvent temperature is harsher.The primary structure of wild silk yarn and spider silk is different from domestic silkworm silk, and the range of choice of its solvent is narrow especially, about the solvent of wild silk yarn and spider silk, there is no so far relevant report.
Summary of the invention
In order to overcome the biological insecurity of the silk-protein solvent that exists in prior art, cost is high and pollution arranged, the deficiencies such as dissolution conditions harshness, the invention provides a kind of method of dissolving silk-protein, this method can not only Simple fast, mild condition ground dissolving natural silk albumen and spun silk fabric, and with low cost, environmentally safe.
A kind of method of dissolving silk-protein of the present invention comprises the following steps:
(1) the 3-10g silk-protein is placed in the 6M-8M urea of 40-60ml after, add 2.5-5g sodium hydrate solid powder, perhaps first after the 6M-8M urea with the 40-60ml of 2.5-5g, again the 3-10g silk-protein is put in mentioned solution, standing 4-24hr under room temperature stirs under room temperature and makes silk protein solution.
Described silk-protein is By Juvenile Hormone, wild silk yarn albumen or spider silk.
Described silk-protein form comprises: silk cocoon silk, degumed silk fiber, waste silk, spun silk fabric.
After the silk protein solution of gained is dialysed, through oven for drying or lyophilize, can obtain the silk-protein powder in distilled water.
The present invention has following advantage:
The present invention is at room temperature take sodium hydroxide and urea soln as solvent, dissolve silk-protein fully, be different from the condition dissolving silk-proteins such as present strong acid, poisonous organic solvent, high temperature fully, and, this invention is not limited to the dissolving By Juvenile Hormone, can also dissolve wild silk yarn albumen and spider silk fibroin.The present invention can be dissolved the silk-protein of various forms: silk cocoon silk, degumed silk fiber, waste silk, spun silk fabric.
The present invention at room temperature can reach silk-protein and dissolve fully take sodium hydroxide, urea, water as raw material, compared to the prior art, consumes energy low, and biological safety is high, and is cheap, simple to operation, environmentally safe.In addition, the easy recycling use of waste liquid, the silk-protein powder of the present invention's preparation can be applicable to the raw material in the fields such as food, makeup, medicine, biomaterial.
Embodiment
The present invention is further described by the following examples:
Example 1
Get the kind in wild silk yarn, tussah silk.With the oven dry of coming unstuck of tussah cocoon boiling water.Get tussah silk fibroin 2.5 grams that come unstuck, put into the 8M urea soln of 50ml, add again 5g sodium hydroxide, be stirred to sodium hydroxide and dissolve fully, under room temperature standing 12 hours, be stirred to tussah silk fibroin and dissolve fully, obtain silk protein solution, after dialysis, lyophilize obtains approximately 2g tussah silk fibroin powder in distilled water.
Example 2
Get silk fibroin protein 3 grams that come unstuck, put into the 8M urea soln of 50ml, add again 5g sodium hydroxide, be stirred to sodium hydroxide and dissolve fully, under room temperature standing 4 hours, be stirred to tussah silk fibroin and dissolve fully, obtain silk protein solution, after dialysis, lyophilize obtains approximately 2.6g silk fibroin protein powder in distilled water.
Example 3
Get spun silk fabric 5g, put into the 8M urea soln of 50ml, add again 8g sodium hydroxide, be stirred to sodium hydroxide and dissolve fully, under room temperature standing 8 hours, be stirred to tussah silk fibroin and dissolve fully, obtain silk protein solution, after dialysis, lyophilize obtains 2g silk fibroin protein powder in distilled water.
At last, it is also to be noted that, what more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.

Claims (2)

1. method of dissolving silk-protein is characterized in that comprising the following steps:
After the 3-10g silk-protein being placed in the 6M-8M urea of 40-60ml, add 2.5-5g sodium hydrate solid powder, after perhaps first the sodium hydrate solid powder of 2.5-5g being dissolved in the 6M-8M urea of 40-60ml, again the 3-10g silk-protein is put in mentioned solution, standing 4-24hr under room temperature stirs under room temperature and makes silk protein solution;
Described silk-protein is By Juvenile Hormone, wild silk yarn albumen or spider silk;
The silk-protein form comprises: silk cocoon silk, degumed silk fiber, waste silk or spun silk fabric.
2. dissolve according to claim 1 the method for silk-protein, it is characterized in that: after silk protein solution is dialysed, through oven for drying or lyophilize, can obtain the silk-protein powder in distilled water.
CN 201010294430 2010-09-27 2010-09-27 Method for dissolving fibroin Active CN102417599B (en)

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CN 201010294430 CN102417599B (en) 2010-09-27 2010-09-27 Method for dissolving fibroin

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CN102417599B true CN102417599B (en) 2013-06-05

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Publication number Priority date Publication date Assignee Title
AU2015367634B2 (en) 2014-12-15 2021-05-20 Teagasc - The Agriculture And Food Development Authority Gastro-resistant microencapsulates, and uses thereof to stimulate in-vivo ileal GLP-1 release in a mammal
EP3042571A1 (en) * 2014-12-15 2016-07-13 Anabio Technologies Limited A solution of denatured pea protein, and uses thereof to form microbeads
CN106749753A (en) * 2017-01-03 2017-05-31 王玲燕 A kind of biological alginate preparation method
CN110639050A (en) * 2019-10-30 2020-01-03 重庆医科大学 Silk fibroin nanofiber and preparation method of silver-loaded antibacterial dressing based on silk fibroin nanofiber

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1407992A (en) * 1999-12-09 2003-04-02 独立行政法人农业生物资源研究所 Process for producing functional silk fibroin and utilization of the same

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Publication number Priority date Publication date Assignee Title
JPH0790182A (en) * 1993-09-22 1995-04-04 Kanebo Ltd Silk fibroin excellent in shelf stability and its production
JP5604294B2 (en) * 2008-03-26 2014-10-08 倉敷紡績株式会社 Protein separation method, protein dissolution method, non-animal fiber fraction collection method, and animal fiber-derived protein

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1407992A (en) * 1999-12-09 2003-04-02 独立行政法人农业生物资源研究所 Process for producing functional silk fibroin and utilization of the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JP特开平7-90182A 1995.04.04

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