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Method of preparing insoluble fibroin protein film

A silk fibroin, soluble technology, which is applied in the field of preparation of insoluble silk fibroin membranes, can solve the problems of high dissolution loss rate of pure silk fibroin membranes, decreased biocompatibility of silk fibroin mixed membranes, etc., and achieves low cost, biological The effect of good compatibility and simple production process

Inactive Publication Date: 2008-08-06
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the disadvantages of the prior art that the dissolution rate of pure silk fibroin film in water is too high, and blending with other polymer materials causes the biocompatibility of silk fibroin mixed film to decrease

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 1 Put 20g of the cocoon layer into 400mL of 0.5% neutral soap solution, treat it at 100±2°C for 2 hours, remove all the sericin wrapped on the silk fibroin, and obtain silk fibroin after fully washing.

[0012] 2 Place the dried silk fibroin in 250mL of CaCl 2 : C 2 h 5 OH:H 2 In a mixed solution of O=1:2:8 (molar ratio), dissolve in a water bath at 75±2°C for 2 hours. After cooling, filter the crude silk fibroin solution to remove insoluble matter, put it into a cellulose dialysis membrane, dialyze with deionized water for 3 days to remove ions and small silk fibroin molecules, and obtain a regenerated silk fibroin protein solution.

[0013] 3 Measure 10 mL of butyl titanate into 100 mL of ethanol with a dry pipette in a fume hood, and stir magnetically for 30 min. Measure 150mL of silk fibroin solution in a beaker, press TiO 2 : The ratio of silk fibroin=0.4 / 100 (weight percent, the same below) pipettes a quantitative butyl titanate / ethanol solution, slowly adds ...

Embodiment 2

[0016] 1 Put 20g of the cocoon layer into 400mL of 0.5% neutral soap solution, treat it at 100±2°C for 2 hours, remove all the sericin wrapped on the silk fibroin, and obtain silk fibroin after fully washing.

[0017] 2 Place the dried silk fibroin in 250mL of CaCl 2 : C 2 h 5 OH:H 2 In a mixed solution of O=1:2:8 (molar ratio), dissolve in a water bath at 75±2°C for 2 hours. After cooling, filter the crude silk fibroin solution to remove insoluble matter, put it into a cellulose dialysis membrane, dialyze with deionized water for 3 days to remove ions and small silk fibroin molecules, and obtain a regenerated silk fibroin protein solution.

[0018] 3 Use a dry pipette to measure 10mL butyl titanate into 100mL ethanol in a fume hood, stir magnetically for 45min, measure 150mL silk fibroin solution into a beaker, press TiO 2 : The ratio of silk fibroin=0.6 / 100 pipettes quantitative butyl titanate / ethanol solution, slowly adds in the silk fibroin solution, adjusts the pH val...

Embodiment 3

[0021] 1 Put 20g of the cocoon layer into 400mL of 0.5% neutral soap solution, treat it at 100±2°C for 2 hours, remove all the sericin wrapped on the silk fibroin, and obtain silk fibroin after fully washing.

[0022] 2 Place the dried silk fibroin in 250mL of CaCl 2 : C 2 h 5 OH:H 2 In a mixed solution of O=1:2:8 (molar ratio), dissolve in a water bath at 75±2°C for 2 hours. After cooling, filter the crude silk fibroin solution to remove insoluble matter, put it into a cellulose dialysis membrane, dialyze with deionized water for 3 days to remove ions and small silk fibroin molecules, and obtain a regenerated silk fibroin protein solution.

[0023] 3 Use a dry pipette to measure 10mL butyl titanate into 100mL ethanol in a fume hood, stir magnetically for 60min, measure 150mL silk fibroin solution into a beaker, press TiO 2 : Silk fibroin=0.8 / 100 ratio Pipette quantitative butyl titanate / ethanol solution, slowly add into the silk fibroin solution, adjust the pH value to 5....

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Abstract

The invention discloses a preparation method for an insoluble silk fibroin membrane, and the preparation steps are as follows: obtaining the pure silk fibroin solution through the degumming, dissolution, dialysis and purification of the silk; mixing and stirring butyl titanate and ethanol with the volume ratio of 1 : 10, and adding the generated nanometer TiO2 and silk with the weight percentage of 0.4 to 0.8 percent into the pure silk solution, and adjusting the pH value as 5 to 6, and making magnetic stirring; the solution is dried into a membrane in the condition of a temperature of 20 to 40 DEG C and the relative humidity of 40 to 80 percent. The silk fibroin membrane of the invention is provided with no toxicity or harm and has good biocompatibility; the structure of the silk is a non crystalline state; the silk membrane has the water dissolve-loss rate of less than 2 percent, the elongation breaking strength of 50 to 80M / Pa, the breaking elongation rate of less than 40 percent and the amount of water transmission of 120 to 250g / (m<2>*h); meanwhile, the silk fibroin membrane is insoluble in water and only needs small amount of nanometer particles. The silk fibroin membrane is simple in preparation, low in cost and can be used in materials such as wound protective membranes, artificial skin, anticoagulant materials, ligaments, vessels, tendons and drug controlling.

Description

technical field [0001] The invention relates to a preparation method of a silk fibroin film, in particular to a preparation method of an insoluble silk fibroin film. Background technique [0002] Silk is a natural polymer material. Silk fibroin accounts for 70-80% of silk and is obtained by degumming silk. Silk fibroin has good biocompatibility and degradability with the human body, and has a wide range of applications in the biological field. . The silk film made from silk fibroin can be used as artificial skin, anticoagulant material, drug controlled release material, etc. The silk fibroin film prepared by pure silk fibroin solution has high water solubility and low strength, and the dissolution rate of silk fibroin film can be reduced and the strength of silk fibroin film can be improved by methanol treatment, but the silk fibroin film obtained is relatively brittle and has low strength , lower elongation at break. In order to improve the performance of silk fibroin fi...

Claims

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Application Information

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IPC IPC(8): A61L15/32A61L27/22A61L27/60A61L33/12A61K47/42C08L89/00C08K3/22C08J5/18
Inventor 冯新星陈建勇朱海霖张建春郭玉海张华鹏
Owner ZHEJIANG SCI-TECH UNIV
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