CN103160946A - Preparation method of tissue engineering scaffold fibrous material - Google Patents
Preparation method of tissue engineering scaffold fibrous material Download PDFInfo
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- CN103160946A CN103160946A CN 201110414689 CN201110414689A CN103160946A CN 103160946 A CN103160946 A CN 103160946A CN 201110414689 CN201110414689 CN 201110414689 CN 201110414689 A CN201110414689 A CN 201110414689A CN 103160946 A CN103160946 A CN 103160946A
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Abstract
The present invention discloses a preparation method of tissue engineering scaffold fibrous material. Silk is used as the main raw material, therefore the obtained regenerated silk fibroin protein fiber has the advantages of good biocompatibility between natural silk fibroin protein and human bodies. Because aggregation structure parameters including crystallinity, orientation degree, etc. of the regenerated silk fibroin protein fiber are controlled in the spinning process, the regenerated silk fibroin protein fiber is biodegradable and becomes an ideal material used for tissue engineering scaffolds.
Description
Technical field
The invention belongs to the organizational engineering technical field, be specifically related to a kind of preparation method of tissue engineering bracket fibrous material.
Background technology
Organizational project is the emerging interdisciplinary field that grows up in the last thirty years, and its final purpose is to produce for recovering, keep or promote the product of human body damaged organ or institutional framework and function, such as organization engineering skin, bone, cartilage, tendon etc.Silk is by approximately 75% fibroin and 25% silk gum are formed, it is quite pure natural protein fiber, to the human body avirulence, have no stimulation, the amino acid of fibroin forms with human collagen albumen certain similitude, having good biocompatibility, is the comparatively desirable raw material of preparation bio-medical goods.But prove after deliberation, because natural silk degree of crystallinity is higher, in crystal region, the adhesion such as large intramolecule hydrogen bond of silk is stronger, space structure is tight, therefore, general silk product is difficult to be biodegradable, and this just makes natural fibroin in the application of biomedical sector, especially be used as the application of tissue engineering material, be greatly limited.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of easy and simple to handle, safe and reliable tissue engineering bracket fibrous material.
The technical solution adopted in the present invention is:
A kind of preparation method of tissue engineering bracket fibrous material is characterized in that comprising the steps:
1) with natural silk degumming, obtain pure natural silk, then with the dissolving of pure natural silk, make silk concentration after purification at 10% 40% spinning solution;
2) be that 55 99% organic solvent or concentration are that 30 60% high-hydroscopicity salt is prepared into solidification liquid with concentration, with spinning solution spinning in coagulating bath, obtain the spun filament cellulose fiber after cleaning;
3) be that 40 90% organic solvent or concentration are that 20 50% high-hydroscopicity salt is prepared into drawing-off liquid with concentration, the spun filament cellulose fiber in bathing, is carried out once in drawing-off or the drawing-off once, its draft speed is 10 100 m/mins, the drawing-off multiplying power is 0.5 20 times, drawing temperature is 50 120 ℃, degree of crystallinity is 0 40 ℃, thereby obtains biodegradable tissue engineering bracket regenerated fibroin fiber.
In described pure natural silk dissolution process, solvent is 65 85% phosphoric acid, and dissolving is 12 48 hours under the temperature conditions of 20 40 ℃.
Described fibroin dissolution process, the ternary solution that solvent is mixed with for the ratio in proportion lithium bromide 35 50%, ethanol 45 55%, water 5 10%, dissolving is 35 hours under the temperature conditions of 60 90 ℃.
Organic solvent in described solidification liquid, drawing-off liquid is a kind of in methyl alcohol, ethanol; The high-hydroscopicity salt is a kind of in ammonium acetate, sodium acetate, ammonium sulfate, sodium sulphate.
Described spinning process condition is to be spinning in the coagulating bath of 20 50 ℃ with spinning solution in temperature, and nitrogen pressure is 0.1Mpa 0.5Mpa, and the spinning plate aperture is 0.2mm 0.8mm, and spinning speed is 2 30m/min.
The beneficial effect that technical solution of the present invention is brought is:
The present invention is due to take silk as main raw material, therefore, the regenerated silk fibroin fiber that makes have advantages of natural fibroin protein and the human-body biological compatibility good; Simultaneously, due in aggregated structure parameters such as the degree of crystallinity of controlling the regenerated silk fibroin fiber in spinning process, the degrees of orientation, make regenerated silk fibroin fiber biological degradable, become tissue engineering bracket with desirable fibrous material.
The specific embodiment:
The invention is further illustrated by the following examples, but the present invention is not limited to this.
Embodiment 1
First 0.6 kilogram of leftover bits and pieces raw silk (byproduct in Reeling Silk Mill silk cocoon filature) is put into 10 liters of concentration and be 0.05% aqueous sodium carbonate, boiled 0.5 hour, the silk gum of most fibroin periphery is taken off in reprocessing three times, obtains pure natural silk.
Pure natural silk after naturally drying is 80% phosphoric acid with 1.5 liters of concentration, and dissolving is 2 hours under the temperature conditions of 30 ℃, purifies after filtration, the ultrasonic wave froth breaking makes spinning solution after 1 hour;
Under the effect of 0.4Mpa nitrogen, with the aperture spinneret orifice that is 0.5mm, under the temperature conditions of 25 ℃, speed ejection fibroin albumen spinning solution with 2 grams per minute, entering concentration is in 25% ammonium sulfate solidification liquid, and the temperature of coagulating bath is 30 ℃, and spinning is frozen into nascent fibroin fiber.Nascent fibroin fiber after washing is immersed the first drawing-off bathe, degree of draft is 1 times; Immerse the second drawing-off again and bathe, degree of draft is 2 times.The drawing-off liquid of first and second time drawing-off is the methyl alcohol of concentration 60%, and drawing temperature is 80 ℃.
At last, batch with the speed of 80 meters per minute, make tissue engineering bracket regenerated silk fibroin fiber, its fibroin content is 100%, measures through X-ray diffraction, and its degree of crystallinity is 3%, fibre length is more than 1 meter, fiber number 1dtex, tensile break strength 0.5CN/ dtex.
Embodiment 2
It is 0.5% neutral soap solution that 1 kilogram of cocoon layer is put into 20 liters of concentration, boils 2 hours, takes off the silk gum of most fibroin periphery, obtains pure natural silk after hot water fully washs.
Dried pure natural silk, be lithium bromide, the ethanol of 44: 50: 6, the ternary solution of water with 1.5 liter weight ratios, stirred 4 hours under the temperature conditions of 75 ℃, be dissolved into the fibroin mixed solution, purify after filtration, the ultrasonic wave froth breaking was made spinning solution after 1.5 hours.
Under the effect of 03Mpa nitrogen, be 2 of the spinneret orifices of 0.5mm with the aperture, under 30 ℃ of temperature conditions, with the speed ejection fibroin albumen spinning solution of 3 grams per minute, enter 20 ℃ of methanol concentrations and be in 60% solidification liquid, be frozen into nascent fibroin fiber.
Immerse the first drawing-off and bathe after washing, drawing-off liquid is 15% ammonium acetate solution, and temperature is that 70 ℃ of degree of drafts are more than 1.5 times; Immerse the second drawing-off again and bathe, drawing temperature is 80 ℃, and drawing-off liquid is 10% ammonium acetate solution, and degree of draft is more than 2.0 times.
Batch with the speed of 90 meters per minute at last, make fibroin content and be 95%, degree of crystallinity is 6% tissue engineering bracket regenerated silk fibroin fiber.
Tissue engineering bracket fibroin fiber provided by the invention has kept the protein composition of natural fibroin, has good biocompatibility, and with low cost.Particularly its biodegradability reaches the plasticity of being processed into the used in tissue engineering three-dimensional rack by rear road, be expected as replacing the expensive biodegradable tissue engineering materials such as import PLA, as artificial skin, tissue engineering rack material or the surgical repair materials such as tendon, blood vessel, cartilage, ligament, esophagus, endocranium.
Claims (5)
1. the preparation method of a tissue engineering bracket fibrous material, is characterized in that comprising the steps:
1) first with natural silk degumming, obtain pure natural silk, then with the dissolving of pure natural silk, make silk concentration after purification at 10% 40% spinning solution;
2) be that 55 99% organic solvent or concentration are that 30 60% high-hydroscopicity salt is prepared into solidification liquid with concentration, with spinning solution spinning in coagulating bath, obtain the spun filament cellulose fiber after cleaning;
3) be that 40 90% organic solvent or concentration are that 20 50% high-hydroscopicity salt is prepared into drawing-off liquid with concentration, the spun filament cellulose fiber in bathing, is carried out once in drawing-off or the drawing-off once, its draft speed is 10 100 m/mins, the drawing-off multiplying power is 0.5 20 times, drawing temperature is 50 120 ℃, degree of crystallinity is 0 40 ℃, thereby obtains biodegradable tissue engineering bracket regenerated fibroin fiber.
2. preparation method according to claim 1, it is characterized in that: in described pure natural silk dissolution process, solvent is 65 85% phosphoric acid, dissolving is 12 48 hours under the temperature conditions of 20 40 ℃.
3. preparation method according to claim 1, it is characterized in that: described fibroin dissolution process, the ternary solution that solvent is mixed with for the ratio in proportion lithium bromide 35 50%, ethanol 45 55%, water 5 10%, dissolving is 35 hours under the temperature conditions of 60 90 ℃.
4. preparation method according to claim 1 is characterized in that: the organic solvent in described solidification liquid, drawing-off liquid is a kind of in methyl alcohol, ethanol; The high-hydroscopicity salt is a kind of in ammonium acetate, sodium acetate, ammonium sulfate, sodium sulphate.
5. preparation method according to claim 1, it is characterized in that: described spinning process condition is to be spinning in the coagulating bath of 20 50 ℃ with spinning solution in temperature, and nitrogen pressure is 0.1Mpa 0.5Mpa, the spinning plate aperture is 0.2mm 0.8mm, and spinning speed is 2 30m/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110414689 CN103160946A (en) | 2011-12-13 | 2011-12-13 | Preparation method of tissue engineering scaffold fibrous material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110414689 CN103160946A (en) | 2011-12-13 | 2011-12-13 | Preparation method of tissue engineering scaffold fibrous material |
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| CN103160946A true CN103160946A (en) | 2013-06-19 |
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| CN 201110414689 Withdrawn CN103160946A (en) | 2011-12-13 | 2011-12-13 | Preparation method of tissue engineering scaffold fibrous material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320886A (en) * | 2013-07-15 | 2013-09-25 | 苏州大学 | Bionic regenerated silk fibroin filament fiber and preparation method thereof |
| CN107287686A (en) * | 2017-06-06 | 2017-10-24 | 青岛大学 | A kind of electrically conductive filament and preparation method thereof |
| WO2018028224A1 (en) * | 2016-08-08 | 2018-02-15 | 南通大学 | Silk fibroin with different degradation velocity and use thereof |
-
2011
- 2011-12-13 CN CN 201110414689 patent/CN103160946A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320886A (en) * | 2013-07-15 | 2013-09-25 | 苏州大学 | Bionic regenerated silk fibroin filament fiber and preparation method thereof |
| WO2018028224A1 (en) * | 2016-08-08 | 2018-02-15 | 南通大学 | Silk fibroin with different degradation velocity and use thereof |
| CN107287686A (en) * | 2017-06-06 | 2017-10-24 | 青岛大学 | A kind of electrically conductive filament and preparation method thereof |
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Application publication date: 20130619 |