CN103585674A - Method for preparing porous fibrous scaffold from silk fibroin - Google Patents
Method for preparing porous fibrous scaffold from silk fibroin Download PDFInfo
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- CN103585674A CN103585674A CN201310548929.3A CN201310548929A CN103585674A CN 103585674 A CN103585674 A CN 103585674A CN 201310548929 A CN201310548929 A CN 201310548929A CN 103585674 A CN103585674 A CN 103585674A
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- silk fibroin
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Abstract
The invention provides a method for preparing a porous fibrous scaffold from silk fibroin. The method adopts a thermally induced phase separation method, and comprises the following concrete steps: mixing silk fibroin and another polymer at the mass ratio of (10:0) to (2:8), and under the action of a diluent, sequentially performing polymer solution preparation, gradient cooling, freeze forming, diluent extracting and vacuum freeze drying to obtain the porous fibrous scaffold prepared from the silk fibroin, wherein the diluent is a solution formed through mixing hexafluoroisopropanol and water at the volume ratio of (4:1) to (2:3); the another polymer is one of synthetic materials such as polyethylene, polypropylene, polyurethane, polylactic acid, polylactic acid-glycollic acid and polyphenylene sulfide; the cooling gradient is 25-80 DEG C; the extractant is one of methanol, ethanol and n-hexane. The porous fibrous scaffold prepared from the silk fibroin has favorable biocompatibility and biodegradability.
Description
[technical field]
The present invention relates to a kind of preparation method of silk fibroin porous fibrous framework.
[background technology]
In recent decades, organizational project is arisen at the historic moment as an emerging cross discipline, for simulating structure, physics and the morphological characteristic of natural tissues, replaces human lesion tissue and defective tissue.
At present, weaver's engineering support builds and to comprise that supporting structure, materials and methods etc. are still a significant challenge of organizational project, not only to make support be beneficial to cell propagation, stick and inwardly growth, to promote the transportation of nutrient substance and metabolite simultaneously.
Thermic (TIPS) method that is separated is a kind of method (the US patent1981 that causes being separated to prepare micropore bracket by changing temperature being proposed by Castro, 4 (247): 498), it can control aperture and the pattern of support well, be beneficial to the parcel of cell, and (Acta Biomaterialia easy and simple to handle, 2011,7 (4): 1542 – 1549).At present, thermally induced phase separation is for the production of (Acta Biomaterialia, 2011,7 (4): 1542 – 1549 such as the support of high porosity, support, microspheres; Acta Biomaterialia, 2008,4 (2): 264 – 272; Biomaterials, 2004,25 (12): 2319 – 2329), but there is no bibliographical information for the preparation of fibroin albumen support.And this patent utilizes fibroin albumen and another kind of polymer to prepare porous fibre support for material first, and for organizational project.
[summary of the invention]
The technical problem to be solved in the present invention, is to provide a kind of preparation method of silk fibroin porous fibrous framework, and the silk fibroin porous fibrous framework of preparation has good biocompatibility and biodegradable.
The present invention is achieved in that
A preparation method for silk fibroin porous fibrous framework, described preparation method adopts thermally induced phase separation, and concrete steps are as follows:
Fibroin albumen is mixed with the mass ratio of another kind of polymer with 10:0～2:8, under the effect of diluent, after polymer solution preparation, gradient cooling, freeze forming, extraction diluent and vacuum lyophilization, obtain silk fibroin porous fibrous framework successively; The described diluent solution that to be hexafluoroisopropanol and water be mixed into the volume ratio of 4:1～2:3; The thermograde of described cooling is 25 ℃～-80 ℃; Described extractant is a kind of in methanol, ethanol, hexane; Described synthetic material is a kind of in polyethylene, polypropylene, polyurethane, polylactic acid, polylactic acid-glycollic acid, polyphenylene sulfide.
Freezing shaping when further, described fibroin albumen and another kind of polymer dissolution are in the diluent that hexafluoroisopropanol and water mix.
Further, the backing thickness of described silk fibroin porous fibrous framework is 0.20～0.30mm, and aperture is 0～100 μ m, and fibre diameter is 0.06～10 μ m, and mean porosities is 70%～90%.
Tool of the present invention has the following advantages:
Silk fibroin porous fibrous framework prepared by the present invention is the compound loose structure of nanofiber and micrometer fibers, and it has good biocompatibility and biodegradable.
[specific embodiment]
The present invention relates to a kind of preparation method of silk fibroin porous fibrous framework, described preparation method adopts thermally induced phase separation, and concrete steps are as follows:
Fibroin albumen is mixed with the mass ratio of another kind of polymer with 10:0～2:8, under the effect of diluent, after polymer solution preparation, gradient cooling, freeze forming, extraction diluent and vacuum lyophilization, obtain silk fibroin porous fibrous framework successively; The described diluent solution that to be hexafluoroisopropanol and water be mixed into the volume ratio of 4:1～2:3; Described another kind of polymer is that synthetic material is a kind of in polyethylene, polypropylene, polyurethane, polylactic acid, polylactic acid-glycollic acid, polyphenylene sulfide, can use thermic phase disengagement method support processed; The thermograde of described cooling is 25 ℃～-80 ℃; Described extractant is a kind of in methanol, ethanol, hexane.
The freezing shaping in the diluent that hexafluoroisopropanol and water mix time of described fibroin albumen and another kind of polymer dissolution.
The backing thickness of described silk fibroin porous fibrous framework is 0.20～0.30mm, and aperture is 0～100 μ m, and fibre diameter is 0.06～10 μ m, and mean porosities is 70%～90%.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment mono-:
Preparation 10%(w/v) polymer/(HFIP+ water) solution: get in the HFIP that a certain amount of fibroin albumen is dissolved in certain volume, magnetic agitation makes fibroin albumen polymer dissolution complete, dropwise add afterwards another kind of diluent-distilled water (volume ratio of HFIP and distilled water is 4:1), magnetic agitation is to forming uniform solution simultaneously.
Polymer/(HFIP+ water) solution is taken out and is laid in politef mould, respectively at 25 ℃ of room temperatures, 4 ℃ ,-20 ℃ ,-80 ℃, carry out gradient cooling, after a period of time, using methanol as extractant, join and in mould, process 6h, last lyophilization, obtains silk fibroin porous fibrous framework.
Embodiment bis-:
Preparation 10%(w/v) polymer/(HFIP+ water) solution: fibroin albumen and polypropylene be take to the ratio that mass ratio is 8:2 and take, the HFIP that adds certain volume, magnetic agitation makes polymer dissolution complete, dropwise add afterwards another kind of diluent-distilled water (volume ratio of HFIP and distilled water is 3:1), magnetic agitation is to forming uniform solution simultaneously.
Polymer/(HFIP+ water) solution is taken out and is laid in politef mould, respectively at 25 ℃ of room temperatures, 4 ℃ ,-20 ℃ ,-50 ℃, carry out gradient cooling, after a period of time, using dehydrated alcohol as extractant, join and in mould, process 6h, last lyophilization, obtains silk fibroin porous fibrous framework.
Embodiment tri-:
Preparation 9%(w/v) polymer/(HFIP+ water) solution: fibroin albumen and polyurethane be take to the ratio that mass ratio is 2:8 and take, the HFIP that adds certain volume, magnetic agitation makes polymer dissolution complete, dropwise add afterwards another kind of diluent-distilled water (volume ratio of HFIP and distilled water is 3:1), magnetic agitation is to forming uniform solution simultaneously.
Polymer/(HFIP+ water) solution is taken out and is laid in politef mould, respectively at room temperature, 4 ℃ ,-20 ℃, carry out gradient cooling, after a period of time, join in mould process 6h using ethanol as extractant, lyophilization afterwards, obtains silk fibroin porous fibrous framework.
Embodiment tetra-:
Preparation 9%(w/v) polymer/(HFIP+ water) solution: fibroin albumen and polylactic acid be take to the ratio that mass ratio is 5:5 and take, the HFIP that adds certain volume, magnetic agitation makes polymer dissolution complete, dropwise add afterwards another kind of diluent-distilled water (volume ratio of HFIP and distilled water is 2:1), magnetic agitation is to forming uniform solution simultaneously.Polymer solution is taken out and to be laid in politef mould, respectively at room temperature, 4 ℃ ,-50 ℃, carry out gradient cooling, after a period of time, join in mould process 6h using methanol as extractant, postlyophilization is just prepared porous nano-fibre support.
Embodiment five:
Preparation 8%(w/v) polymer/(HFIP+ water) solution: fibroin albumen and polylactic acid-glycollic acid be take to the ratio that mass ratio is 0:10 and take, the HFIP that adds certain volume, magnetic agitation makes polymer dissolution complete, dropwise add afterwards another kind of diluent-distilled water (volume ratio of HFIP and distilled water is 3:1), magnetic agitation is to forming uniform solution simultaneously.
Polymer/(HFIP+ water) solution is taken out and is laid in politef mould, respectively at room temperature, 4 ℃ ,-80 ℃, carry out gradient cooling, after a period of time, using methanol as extractant, join in mould and process 6h, postlyophilization, obtains silk fibroin porous fibrous framework.
Embodiment six:
Preparation 8%(w/v) polymer/(HFIP+ water) solution: fibroin albumen and polyphenylene sulfide be take to the ratio that mass ratio is 2:8 and take, the HFIP that adds certain volume, magnetic agitation makes polymer dissolution complete, dropwise add afterwards another kind of diluent-distilled water (volume ratio of HFIP and distilled water is 2.25:1), magnetic agitation is to forming uniform solution simultaneously.
Polymer/(HFIP+ water) solution is taken out and is laid in politef mould, respectively at room temperature, 4 ℃ ,-80 ℃, carry out gradient cooling, after a period of time, using ethanol as extractant, join in mould and process 6h, postlyophilization, obtains silk fibroin porous fibrous framework.
Silk fibroin porous fibrous framework prepared by the present invention is the compound loose structure of nanofiber and micrometer fibers, and it has good biocompatibility and biodegradable.
Although more than described the specific embodiment of the present invention; but being familiar with those skilled in the art is to be understood that; our described specific embodiment is illustrative; rather than for the restriction to scope of the present invention; those of ordinary skill in the art are in equivalent modification and the variation done according to spirit of the present invention, all should be encompassed in the scope that claim of the present invention protects.
Claims (3)
1. a preparation method for silk fibroin porous fibrous framework, is characterized in that: described preparation method adopts thermally induced phase separation, and concrete steps are as follows:
Fibroin albumen is mixed with the mass ratio of another kind of polymer with 10:0-2:8, under the effect of diluent, after polymer solution preparation, gradient cooling, freeze forming, extraction diluent and vacuum lyophilization, obtain silk fibroin porous fibrous framework successively; The described diluent solution that to be hexafluoroisopropanol and water be mixed into the volume ratio of 4:1～2:3; The thermograde of described cooling is 25 ℃～-80 ℃; Described extractant is a kind of in methanol, ethanol, hexane; Described another kind is polymerized to a kind of in synthetic material polyethylene, polypropylene, polyurethane, polylactic acid, polylactic acid-glycollic acid, polyphenylene sulfide.
2. according to the preparation method of a kind of silk fibroin porous fibrous framework described in right 1, it is characterized in that: the freezing shaping in the diluent that hexafluoroisopropanol and water mix time of described fibroin albumen and another kind of polymer dissolution.
3. according to the preparation method of a kind of silk fibroin porous fibrous framework described in right 2, it is characterized in that: the backing thickness of described silk fibroin porous fibrous framework is 0.20～0.30mm, aperture is 0～100 μ m, and fibre diameter is 0.06～10 μ m, and mean porosities is 70%～90%.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104383598A (en) * | 2014-12-04 | 2015-03-04 | 湖北赛罗生物材料有限责任公司 | Bioactive material as well as preparation method and application thereof |
| CN106075591A (en) * | 2016-07-12 | 2016-11-09 | 东华大学 | A kind of enhancing lamella composite and preparation method thereof |
| CN106117502A (en) * | 2016-08-05 | 2016-11-16 | 郭迎庆 | A kind of preparation method of medical macromolecular materials |
| CN106178115A (en) * | 2016-07-19 | 2016-12-07 | 福建工程学院 | A kind of high porosity high connectivity biological support preparation method |
| EP3315147A1 (en) * | 2016-10-28 | 2018-05-02 | Bioengineering Laboratories S.r.l. | Hybrid scaffold suitable for regenerating tissues and production process |
| CN108553689A (en) * | 2018-04-13 | 2018-09-21 | 浙江大学 | A kind of fibroin porous microsphere and preparation method thereof with nanofiber micro-structure |
| CN109316633A (en) * | 2016-08-19 | 2019-02-12 | 苏州大学 | A kind of fibroin albumen micro nanometer fiber porous support and its application |
| CN110774680A (en) * | 2019-11-06 | 2020-02-11 | 王娟 | Antibacterial fabric with high skin affinity and preparation method thereof |
| WO2020041381A1 (en) * | 2018-08-20 | 2020-02-27 | Trustees Of Tufts College | Systems and methods for 3d printing of proteins |
| CN113144289A (en) * | 2021-04-27 | 2021-07-23 | 武汉理工大学 | Silk fibroin/polylactic acid composite scaffold with function of directionally inducing peripheral nerve regeneration and preparation method thereof |
| CN114732949A (en) * | 2022-03-25 | 2022-07-12 | 上海工程技术大学 | Rotator cuff patch with oriented structure and preparation method thereof |
| CN115581816A (en) * | 2022-10-09 | 2023-01-10 | 深圳先进技术研究院 | Biological activity multi-stage structure guided tissue regeneration membrane and preparation method thereof |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104383598B (en) * | 2014-12-04 | 2016-02-17 | 湖北赛罗生物材料有限责任公司 | A kind of bioactive materials, its preparation method and application |
| CN104383598A (en) * | 2014-12-04 | 2015-03-04 | 湖北赛罗生物材料有限责任公司 | Bioactive material as well as preparation method and application thereof |
| CN106075591B (en) * | 2016-07-12 | 2019-05-24 | 东华大学 | A kind of enhancing lamella composite material and preparation method |
| CN106075591A (en) * | 2016-07-12 | 2016-11-09 | 东华大学 | A kind of enhancing lamella composite and preparation method thereof |
| CN106178115A (en) * | 2016-07-19 | 2016-12-07 | 福建工程学院 | A kind of high porosity high connectivity biological support preparation method |
| CN106117502A (en) * | 2016-08-05 | 2016-11-16 | 郭迎庆 | A kind of preparation method of medical macromolecular materials |
| CN109316633A (en) * | 2016-08-19 | 2019-02-12 | 苏州大学 | A kind of fibroin albumen micro nanometer fiber porous support and its application |
| CN109316633B (en) * | 2016-08-19 | 2020-12-08 | 苏州大学 | Silk fibroin micro-nanofiber porous scaffold and application thereof |
| WO2018077475A1 (en) | 2016-10-28 | 2018-05-03 | Bioengineering Laboratories S.R.L. | Hybrid scaffold suitable for regenerating animal tissues and process for producing the scaffold |
| EP3315147A1 (en) * | 2016-10-28 | 2018-05-02 | Bioengineering Laboratories S.r.l. | Hybrid scaffold suitable for regenerating tissues and production process |
| US11213612B2 (en) | 2016-10-28 | 2022-01-04 | Dialybrid S.r.l. | Hybrid scaffold suitable for regenerating animal tissues and process for producing the scaffold |
| EP3799892A1 (en) | 2016-10-28 | 2021-04-07 | Dialybrid S.r.l. | Hybrid scaffold suitable for regenerating animal tissues and process for producing the scaffold |
| CN108553689A (en) * | 2018-04-13 | 2018-09-21 | 浙江大学 | A kind of fibroin porous microsphere and preparation method thereof with nanofiber micro-structure |
| CN108553689B (en) * | 2018-04-13 | 2020-03-27 | 浙江大学 | Silk fibroin porous microsphere with nanofiber microstructure and preparation method thereof |
| WO2020041381A1 (en) * | 2018-08-20 | 2020-02-27 | Trustees Of Tufts College | Systems and methods for 3d printing of proteins |
| CN110774680A (en) * | 2019-11-06 | 2020-02-11 | 王娟 | Antibacterial fabric with high skin affinity and preparation method thereof |
| CN113144289A (en) * | 2021-04-27 | 2021-07-23 | 武汉理工大学 | Silk fibroin/polylactic acid composite scaffold with function of directionally inducing peripheral nerve regeneration and preparation method thereof |
| CN114732949A (en) * | 2022-03-25 | 2022-07-12 | 上海工程技术大学 | Rotator cuff patch with oriented structure and preparation method thereof |
| CN114732949B (en) * | 2022-03-25 | 2023-01-24 | 上海工程技术大学 | Rotator cuff patch with oriented structure and preparation method thereof |
| CN115581816A (en) * | 2022-10-09 | 2023-01-10 | 深圳先进技术研究院 | Biological activity multi-stage structure guided tissue regeneration membrane and preparation method thereof |
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Application publication date: 20140219 |