CN102417599A - Method for dissolving fibroin - Google Patents
Method for dissolving fibroin Download PDFInfo
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- CN102417599A CN102417599A CN2010102944300A CN201010294430A CN102417599A CN 102417599 A CN102417599 A CN 102417599A CN 2010102944300 A CN2010102944300 A CN 2010102944300A CN 201010294430 A CN201010294430 A CN 201010294430A CN 102417599 A CN102417599 A CN 102417599A
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- silk
- protein
- fibroin
- room temperature
- urea
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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
Technical field
The present invention relates to the natural polymer field, particularly a kind of method of dissolving silk-protein.
Background technology
Domestic silkworm silk albumen, wild silk yarn albumen (tussah silk and wild silk yarn etc.) and spider silk are protein fibres; Because of its special mechanical properties and excellent biological compatibility, degradation property and stability; And essence is proteinic constructional feature; Can obtain regenerated silk protein fiber, silk fibroin powder, fibroin protein film, fibroin porous material after treatment, be applied to 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 the sericterium; In becoming the silk process, under the influence 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 competent waste cocoon and waste silk resource are arranged, and how to utilize the reclaiming of inferior horn cocoon, waste silk and spun silk fabric article resource at low cost, and one of gordian technique is exactly to find that cost is low, operational safety is simple and easy, environment amenable solvent.Japan's report (Japan PatentWO2009119596-A1) places domestic silkworm silk albumen the 8M urea soln to heat to 200 ℃, can dissolve silk-protein, but conditions such as solvent temperature are relatively harsher.The primary structure of wild silk yarn and spider silk is different from domestic silkworm silk, and its choice of Solvent scope is narrow especially, about the solvent of wild silk yarn and spider silk, does not have relevant report so far.
Summary of the invention
In order to overcome the biological insecurity of the silk-protein solvent that exists in the prior art; Cost is high and deficiencies such as pollution, dissolution conditions harshness are arranged, and the invention provides a kind of method of dissolving silk-protein; This method can not only be simply quick; 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 may further comprise the steps:
(1) the 3-10g silk-protein is placed the 6M-8M urea of 40-60ml after; Add 2.5-5g sodium hydrate solid powder; Perhaps behind the 6M-8M urea of elder generation with the 40-60ml of 2.5-5g; The 3-10g silk-protein is put in the above-mentioned solution again, leaves standstill 4-24hr under the room temperature, stirring under the room temperature makes silk protein solution.
Described silk-protein is domestic silkworm silk albumen, 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,, can obtain the silk-protein powder through oven for drying or lyophilize in zero(ppm) water.
The present invention has following advantage:
The present invention is a solvent with sodium hydroxide and urea soln at room temperature; Dissolve silk-protein fully; Be different from condition dissolving silk-proteins such as present strong acid, poisonous organic solvent, high temperature fully; And this invention is not limited to dissolving domestic silkworm silk albumen, 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 is a raw material with sodium hydroxide, urea, water, at room temperature can reach silk-protein and dissolve fully, compares with prior art, and it is low to consume energy, and biological safety is high, and is cheap, simple to operation, environmentally safe.In addition, the waste liquid easy recovery recycles, and the silk-protein powder of the present invention's preparation can be applicable to the raw material in fields such as food, makeup, medicine, biomaterial.
Embodiment
Below further present invention is described through embodiment:
Instance 1
Get the kind in the 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 5g sodium hydroxide again; Be stirred to sodium hydroxide and dissolve fully, left standstill under the room temperature 12 hours, be stirred to tussah silk fibroin and dissolve fully; Obtain silk protein solution; After the dialysis, lyophilize obtains about 2g tussah silk fibroin powder in zero(ppm) water.
Instance 2
Get silk fibroin protein 3 grams that come unstuck, put into the 8M urea soln of 50ml, add 5g sodium hydroxide again; Be stirred to sodium hydroxide and dissolve fully, left standstill under the room temperature 4 hours, be stirred to tussah silk fibroin and dissolve fully; Obtain silk protein solution; After the dialysis, lyophilize obtains about 2.6g silk fibroin protein powder in zero(ppm) water.
Instance 3
Get spun silk fabric 5g, put into the 8M urea soln of 50ml, add 8g sodium hydroxide again; Be stirred to sodium hydroxide and dissolve fully, left standstill under the room temperature 8 hours, be stirred to tussah silk fibroin and dissolve fully; Obtain silk protein solution; After the dialysis, lyophilize obtains 2g silk fibroin protein powder in zero(ppm) water.
At last, it is also to be noted that what more than enumerate only is practical implementation example of the present 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 (4)
1. method of dissolving silk-protein is characterized in that may further comprise the steps:
After the 3-10g silk-protein being placed the 6M-8M urea of 40-60ml; Add 2.5-5g sodium hydrate solid powder; After perhaps first sodium hydrate solid powder with 2.5-5g is dissolved in the 6M-8M urea of 40-60ml; The 3-10g silk-protein is put in the above-mentioned solution again, leaves standstill 4-24hr under the room temperature, stirring under the room temperature makes silk protein solution.
2. method according to claim 1 is characterized in that: described silk-protein is domestic silkworm silk albumen, wild silk yarn albumen or spider silk.
3. method according to claim 1 and 2 is characterized in that described silk-protein form comprises: silk cocoon silk, degumed silk fiber, waste silk, spun silk fabric.
4. after the silk protein solution of the arbitrary gained of claim 1 to 3 is dialysed,, can obtain the silk-protein powder through oven for drying or lyophilize in zero(ppm) water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010294430 CN102417599B (en) | 2010-09-27 | 2010-09-27 | Method for dissolving fibroin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010294430 CN102417599B (en) | 2010-09-27 | 2010-09-27 | Method for dissolving fibroin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102417599A true CN102417599A (en) | 2012-04-18 |
| CN102417599B CN102417599B (en) | 2013-06-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010294430 Active CN102417599B (en) | 2010-09-27 | 2010-09-27 | Method for dissolving fibroin |
Country Status (1)
| Country | Link |
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| CN (1) | CN102417599B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749753A (en) * | 2017-01-03 | 2017-05-31 | 王玲燕 | A kind of biological alginate preparation method |
| CN107404899A (en) * | 2014-12-15 | 2017-11-28 | 安纳生物科技有限公司 | It is denatured pea protein solution and its forms the purposes of particulate |
| 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 |
| US11103550B2 (en) | 2014-12-15 | 2021-08-31 | Anabio Technologies Limited | Gastro-resistant microencapsulates, and uses thereof to stimulate in-vivo ileal GLP-1 release in a mammal |
Citations (3)
| 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 |
| 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 |
| WO2009119596A1 (en) * | 2008-03-26 | 2009-10-01 | 国立大学法人岐阜大学 | Method of classifying proteins, method of dissolving proteins, method of fractionating and collecting non-animal fiber and proteins originating in animal fiber |
-
2010
- 2010-09-27 CN CN 201010294430 patent/CN102417599B/en active Active
Patent Citations (3)
| 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 |
| 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 |
| WO2009119596A1 (en) * | 2008-03-26 | 2009-10-01 | 国立大学法人岐阜大学 | Method of classifying proteins, method of dissolving proteins, method of fractionating and collecting non-animal fiber and proteins originating in animal fiber |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107404899A (en) * | 2014-12-15 | 2017-11-28 | 安纳生物科技有限公司 | It is denatured pea protein solution and its forms the purposes of particulate |
| US11103550B2 (en) | 2014-12-15 | 2021-08-31 | Anabio Technologies Limited | Gastro-resistant microencapsulates, and uses thereof to stimulate in-vivo ileal GLP-1 release in a mammal |
| CN107404899B (en) * | 2014-12-15 | 2021-12-07 | 诺比美有限公司 | Denatured pea protein solution and use thereof for forming microparticles |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102417599B (en) | 2013-06-05 |
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