CN101234212A - Method of preparing soluble-high elasticity fibroin protein film - Google Patents
Method of preparing soluble-high elasticity fibroin protein film Download PDFInfo
- Publication number
- CN101234212A CN101234212A CNA2008100598768A CN200810059876A CN101234212A CN 101234212 A CN101234212 A CN 101234212A CN A2008100598768 A CNA2008100598768 A CN A2008100598768A CN 200810059876 A CN200810059876 A CN 200810059876A CN 101234212 A CN101234212 A CN 101234212A
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- China
- Prior art keywords
- percent
- fibroin
- silk fibroin
- preparation
- soluble
- Prior art date
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- 108010022355 Fibroins Proteins 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000004793 Polystyrene Substances 0.000 claims abstract description 6
- 238000000502 dialysis Methods 0.000 claims abstract description 6
- 229920002223 polystyrene Polymers 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 8
- 241000255789 Bombyx mori Species 0.000 claims description 5
- 229920002678 cellulose Polymers 0.000 claims description 5
- 239000001913 cellulose Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 239000012528 membrane Substances 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 2
- 210000003041 ligament Anatomy 0.000 abstract description 2
- 230000008961 swelling Effects 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 108010013296 Sericins Proteins 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000008149 soap solution Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- Materials For Medical Uses (AREA)
Abstract
The invention discloses a preparation method for a soluble-high elastic silk fibroin membrane, and the preparation steps are as follows: firstly the silk is transformed into the pure silk fibroin solution with the weight percentage of 0.5 to 0.8 percent through degumming, dissolution, dialysis, purification and concentration; the purified and concentrated pure silk fibroin solution dries slowly into the silk fibroin membrane with the thickness of 30 to 50Mu m in a constant temperature and constant humidity box with the relative humidity of 60 to 80 percent and a temperature of 40 to 70 DEG C after being injected into a polystyrene culture dish. The soluble high elastic silk fibroin membrane prepared by the invention is provided with no toxicity or harm and has good biocompatibility, the swelling ratio of less than 3 percent for 3 hours in water, the dissolve-loss rate of less than 15 percent in 12 hours, the elongation breaking strength of more than 550N/cm <3>, the breaking elongation ratio of more than 50 percent and the elastic recovery rate of more than 65 percent. The preparation method is simple in process, low in cost and can be widely applied to materials such as wound protective membranes, artificial skin, ligaments and drug controlling.
Description
Technical field
The present invention relates to the preparation method of fibroin protein film, particularly relate to a kind of preparation method of soluble-high elasticity fibroin protein film.
Background technology
Silkworm silk is a kind of natural macromolecular material, and fibroin accounts for 70～80% of silkworm silk, is after silkworm silk comes unstuck and obtain.Fibroin and human body have excellent biological compatibility and degradability, have a wide range of applications at biological field.With the fibroin is the fibroin membrane that raw material makes, and can be used as artificial skin, anticoagulant material, drug controlled release material etc.Common method makes that the fibroin protein film water solublity is big, intensity is low; After the processing of methanol βization, though the water dissolve-loss ratio of film is descended, intensity is improved, owing to also can impact its biological degradability in the βization process.Therefore seek the method for the solvable and flexible fibroin material of a kind of novel preparation, improving fibroin material, to be directly used in biomedical sector be unusual meaning.
Summary of the invention
In order to overcome in the prior art, the big intensity of dissolve-loss ratio is low in the pure silk fibroin film water, after the processing of methanol βization and biodegradation shortcoming slowly, the object of the present invention is to provide the preparation method of the good soluble-high elasticity fibroin protein film of a kind of biocompatibility.
The technical solution used in the present invention is that the step of this method is as follows:
1) earlier with silkworm silk through come unstuck, the pure silk fibroin solution of dissolving, dialysis, purification, simmer down to percentage by weight 0.5%～0.8%;
2) the pure silk cellulose solution that will purify after concentrating injects polystyrene culture dish, is 60～80% at relative humidity, and temperature is slowly to be dried to fibroin protein film in 40～70 ℃ the climatic chamber, and the thickness of film is 30～50 μ m.
Be 1～3 day described slow drying time.
The beneficial effect that the present invention has is:
The solvable high resiliency fibroin membrane that the present invention makes is nontoxic, and biocompatibility is good, and less than 15%, tensile break strength was greater than 550N/cm less than 3%, 12 hour dissolve-loss ratio for 3 hours swelling ratio in water
3, elongation at break is greater than 50%, and elastic restoration ratio is greater than 65%.And processing technology is simple, and is with low cost, can be widely used in materials such as Wound surface protection film, artificial skin, ligament, medicine control.
The specific embodiment
Embodiment 1:
1. the cocoon layer of 20g being put into 400mL concentration is 0.5% neutral soap solution, handles 2h in 100 ± 2 ℃, takes off the sericin that is wrapped in to the greatest extent on the fibroin, obtains fibroin albumen behind the thorough washing.
2. the fibroin albumen after will drying places the CaCl of 250mL
2: C
2H
5OH: H
2O=1: in the mixed solution of 2: 8 (mol ratio), in 75 ± 2 ℃ of water-baths, dissolve 2h.After the cooling the thick solution of fibroin is filtered the removal insoluble matter, the cellulose dialyzer of packing into was removed ion and fibroin micromolecule in 3 days with the deionized water dialysis, was condensed into 0.7% pure regenerated silk solution.
3 with above-mentioned solution injection polystyrene culture dish, is 60% at relative humidity, and temperature is to put into climatic chamber under 50 ℃ of conditions to place 2 days, and drying and forming-film, the thickness of film are 50 μ m.
Embodiment 2:
1 the cocoon layer of 20g is put into 400mL concentration is 0.5% neutral soap solution, handles 2h in 100 ± 2 ℃, takes off the sericin that is wrapped in to the greatest extent on the fibroin, obtains fibroin albumen behind the thorough washing.
2 fibroin albumens after will drying place the CaCl of 250mL
2: C
2H
5OH: H
2O=1: in the mixed solution of 2: 8 (mol ratio), in 75 ± 2 ℃ of water-baths, dissolve 2h.After the cooling the thick solution of fibroin is filtered the removal insoluble matter, the cellulose dialyzer of packing into was removed ion and fibroin micromolecule in 3 days with the deionized water dialysis, was condensed into 0.5% pure regenerated silk solution.
3 with above-mentioned solution injection polystyrene culture dish, is 70% at relative humidity, and temperature is to put into climatic chamber under 40 ℃ of conditions to place 3 days, and drying and forming-film, the thickness of film are 40 μ m.
Embodiment 3:
1 the cocoon layer of 20g is put into 400mL concentration is 0.5% neutral soap solution, handles 2h in 100 ± 2 ℃, takes off the sericin that is wrapped in to the greatest extent on the fibroin, obtains fibroin albumen behind the thorough washing.
2 fibroin albumens after will drying place the CaCl of 250mL
2: C
2H
5OH: H
2O=1: in the mixed solution of 2: 8 (mol ratio), in 75 ± 2 ℃ of water-baths, dissolve 2h.After the cooling the thick solution of fibroin is filtered the removal insoluble matter, the cellulose dialyzer of packing into was removed ion and fibroin micromolecule in 3 days with the deionized water dialysis, was condensed into 0.8% pure regenerated silk solution.
3 with above-mentioned solution injection polystyrene culture dish, is 80% at relative humidity, and temperature is to put into climatic chamber under 70 ℃ of conditions to place 1 day, and drying and forming-film, the thickness of film are 30 μ m.
Claims (2)
1, a kind of preparation method of soluble-high elasticity fibroin protein film is characterized in that the step of this method is as follows:
1) earlier with silkworm silk through come unstuck, the pure silk fibroin solution of dissolving, dialysis, purification, simmer down to percentage by weight 0.5%～0.8%;
2) the pure silk cellulose solution that will purify after concentrating injects polystyrene culture dish, is 60～80% at relative humidity, and temperature is slowly to be dried to fibroin protein film in 40～70 ℃ the climatic chamber, and the thickness of film is 30～50 μ m.
2, the preparation method of a kind of soluble-high elasticity fibroin protein film according to claim 1 is characterized in that: be 1～3 day described slow drying time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100598768A CN101234212A (en) | 2008-02-26 | 2008-02-26 | Method of preparing soluble-high elasticity fibroin protein film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100598768A CN101234212A (en) | 2008-02-26 | 2008-02-26 | Method of preparing soluble-high elasticity fibroin protein film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101234212A true CN101234212A (en) | 2008-08-06 |
Family
ID=39918279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100598768A Pending CN101234212A (en) | 2008-02-26 | 2008-02-26 | Method of preparing soluble-high elasticity fibroin protein film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101234212A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341214A (en) * | 2013-07-08 | 2013-10-09 | 苏州大学 | Silk fibroin membrane and preparation method thereof |
| CN104530454A (en) * | 2014-12-23 | 2015-04-22 | 惠州学院 | Method for preparing silk fibroin-polyethylene oxide composite film |
| TWI670303B (en) * | 2018-11-14 | 2019-09-01 | 國立虎尾科技大學 | Anti-ultraviolet biodegradable transparent film based on bionic structure and method fabricating the same |
| WO2022088521A1 (en) * | 2020-10-29 | 2022-05-05 | 之江实验室 | Method for preparing fibroin film using wet film coating method |
-
2008
- 2008-02-26 CN CNA2008100598768A patent/CN101234212A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341214A (en) * | 2013-07-08 | 2013-10-09 | 苏州大学 | Silk fibroin membrane and preparation method thereof |
| CN104530454A (en) * | 2014-12-23 | 2015-04-22 | 惠州学院 | Method for preparing silk fibroin-polyethylene oxide composite film |
| TWI670303B (en) * | 2018-11-14 | 2019-09-01 | 國立虎尾科技大學 | Anti-ultraviolet biodegradable transparent film based on bionic structure and method fabricating the same |
| WO2022088521A1 (en) * | 2020-10-29 | 2022-05-05 | 之江实验室 | Method for preparing fibroin film using wet film coating method |
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| PB01 | Publication | ||
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Open date: 20080806 |