CN1095497C - Method for preparation of repairing porous frame usedd for tissue and organ by a phase separation filter method - Google Patents
Method for preparation of repairing porous frame usedd for tissue and organ by a phase separation filter method Download PDFInfo
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- CN1095497C CN1095497C CN00105637A CN00105637A CN1095497C CN 1095497 C CN1095497 C CN 1095497C CN 00105637 A CN00105637 A CN 00105637A CN 00105637 A CN00105637 A CN 00105637A CN 1095497 C CN1095497 C CN 1095497C
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- organ
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- dioxane
- pore former
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
Abstract
The present invention relates to a method for preparing a poriferous stent used for repairing tissue and organs, particularly to a phase separation particle filtering method. The present invention comprises: firstly, a biocompatibility polymer is prepared into a solution, pore-forming agents are added in the polymer solution, and the polymer solution are evenly mixed to be poured in a mould to be quenched, processed in a die sinking mode, and dried; then, a freeze drying product is immersed in deionized water; finally, the polymer solution is dried in vacuum. Thereby, the poriferous stent of the present invention can be obtained. The stent material prepared by the present invention has the advantages of high porosity, good biocompatibility and biologic degradability.
Description
The present invention relates to the preparation method of a kind of tissue, organ porous holder for repairing, specially refer to a kind of preparation method of the biodegradable porous support of using as the cell growing carrier, belong to biomedical engineering field.
In recent years, the damaged or nonfunction of tissue, organ has been brought grave danger to human health, makes countless families bear destructive strike.The frequent generation that organ, tissue breakdown are damaged and can supply contradiction between the wretched insufficiency of transplant organ, tissue clinically becomes the bottleneck that the people ' s health level improves day by day.In order to alleviate above-mentioned contradiction, organizational project is by porous support, with this somatocyte in vitro culture various implantable intravital tissues and organ.The used in tissue engineering porous support should meet following requirement: 1) surface energy makes cell adhesion and grows 2) implant after, polymkeric substance and degraded product thereof can not cause inflammation and toxic side effect 3) porous support should have into three-dimensional structure 4) for providing the extracellular regenerated enough spaces, the porous support porosity must not be lower than 90%5) can be absorbed 6 by body immediately finishing tissue regeneration post polymerization thing) degradation rate of porous support should be complementary with different tissues cell proliferation speed.
Tissue, the organ porous holder for repairing had extensive studies abroad, up to the present, roughly the preparation method be summarized as the fibrage method, the solution-cast particle leaches method, melt-processed method, phase separation method, high-pressure carbon dioxide method.Domestic research still is in the starting stage.
The particle that is separated leaches method and has drawn the advantage that the solution-cast particle leaches method, phase separation method, has solved the too little problem in simple phase separation method aperture, and the solution-cast particle leaches the particle precipitation problem that legal system is equipped with three-dimensional material.
The particle that is separated that the present invention proposes leaches the method that legal system is organized fully, organ is used repair porous scaffold, comprises following each step:
1, biocompatible polymer is mixed with solution, wherein polymkeric substance for poly-(3-butyric ester) (PHB), the multipolymer (PLGA) of multipolymer (PHB-HH), poly(lactic acid) (PLA), lactic acid and the oxyacetic acid of 3-butyric ester and 3-hydroxycaproic ester etc., solvent is 1,4-dioxane or 1,4-dioxane: 1 of water=100: 0～15,4-dioxane-water mixture, the mass percent concentration that makes this solution is 5%～25%.
2, get the pore former of particle diameter in 100 microns～400 micrometer ranges by the standard sieve sieve, pore former is sodium-chlor, Repone K, Potassium ethanoate, sodium bicarbonate, yellow soda ash, citric acid, Tripotassium Citrate etc.
3, in the ratio of 1: 9～30 (polymkeric substance-pore former mass ratio), the pore former in 2 is joined in the polymers soln described in 1, stir.
4, stir, the mixture in 3 is poured into quenching in the mould of preset temp, quench temperature is between-180 ℃～11.8 ℃, and quenching time is 5 minutes～2 hours (look the amount of goods and select time, freeze fully get final product).
5, die sinking, in type goods lyophilize, freezing temp is between-130 ℃～11.8 ℃, and drying pressure is at 0.001325MPa～0MPa, sublimation drying two days～four days.
6, the goods with lyophilize in 5 are soaked into poor ionized water, change deionized water, and take out goods after 72 hours in per 8 hours.
7, with goods vacuum-drying in 6, temperature is 37 ℃, and pressure is 0.001325Mpa～0Mpa, dry 24 hours, promptly obtains porous support of the present invention.
Use the method for this patent, the tissue of preparation, organ reparation timbering material have following characteristics and advantage:
(1) porosity can reach more than 90%.
(2) resulting timbering material good biocompatibility, and biodegradable.
(3) directly prepare the timbering material of 3-D solid structure, solved the particle precipitation problem that the solution-cast particle leaches method.
(4) magnitude range in hole promptly has macropore reaching several microns between 300 microns, and aperture is arranged again, has solved the too little problem in simple phase separation method aperture.And be interconnected between macropore-macropore, macropore-aperture, the aperture-aperture (as Fig. 1, as shown in Figure 2) is fit to the growth of all size cell, avoided the closed pore problem of high-pressure carbon dioxide method.
(5) must high-temperature operation, avoided the polymer degradation problem that may cause in the melt-processed method.
Description of drawings:
Fig. 1 is the macropore-macropore relation that leaches the PHB timbering material of method preparation with the particle that is separated of the present invention.
Fig. 2 is aperture-aperture, the macropore-aperture relation that leaches the PHB timbering material of method preparation with the particle that is separated of the present invention.
Fig. 3 leaches the PHB timbering material of method preparation with the particle that is separated of the present invention.
Introduce embodiments of the invention below.
Embodiment 1
1, under 55 ℃, with 1 gram poly-(3-butyric ester) (PHB), 10ml 1 in beaker, and the 4-dioxane is mixed with the PHB solution of 10% (quality is than volume).
2, add 15gNaCl, wherein the NaCl diameter is between 100 microns～400 microns.
3, stir down in-10 ℃ of following quenchings.
4, after freezing 10 minutes, cut the sample of desired shape.
5, in-10 ℃, lyophilize 4 days under 0.001325MPa～0MPa.
6, take out goods, it is immersed deionized water, changed water one time, soaked 3 days in per 8 hours.
7, vacuum-drying is 1 day, and temperature is 37 ℃, and pressure is 0.001325MPa～0MPa.
So tissue, organ porous holder for repairing are promptly made.
Embodiment 2
1, under 60 ℃, with the lactic acid and the co-glycolic acid (PLGA) of 1.5 grams, 10ml 1 in beaker, and the 4-dioxane is mixed with 15% (quality is than volume) PLGA solution.
2, add 22.5g KCl, wherein the KCl diameter is between 100 microns～400 microns.
3, stir that to pour preset temperature down into be quenching in 0 ℃ the mould.
4, after freezing 20 minutes, die sinking obtains the sample of desired shape.
5, in 0 ℃, lyophilize 4 days under 0.001325MPa～0MPa.
6, take out sample, it is immersed deionized water, changed water one time, soaked 3 days in per 8 hours.
7, vacuum-drying is 1 day, and temperature is 37 ℃, and pressure is 0.001325MPa～0MPa.
Tissue, organ porous holder for repairing are promptly made.
Embodiment 3
1, under 55 ℃, in the sub-beaker with 1.5 the gram the 3-butyric esters and the multipolymer (PHB-HH) of 3-hydroxycaproic ester, 10ml 1, and 4-dioxane-water mixture (1,4-dioxane, water volume ratio are 87: 13) is mixed with 15% (quality is than volume) preparation PHB-HH solution.
2, add 22.5g KCl, wherein the NaCl diameter is between 100 microns～400 microns.
3, pour under the stirring with quenching in liquid nitrogen (-170 ℃ approximately) the refrigerative mould.
4, after freezing 20 minutes, die sinking obtains the sample of desired shape.
5, in 0 ℃, lyophilize 4 days under 0.001325MPa～0MPa.
6, take out sample, it is immersed deionized water, changed water one time, soaked 3 days in per 8 hours.
7, vacuum-drying is 1 day, and temperature is 37 ℃, and pressure is 0.001325MPa～0MPa.
Tissue, organ porous holder for repairing are promptly made.
Embodiment 4
1, under 60 ℃, in beaker, select the poly(lactic acid) (PLA) of 1.5 grams for use, 10ml 1,15% one-tenth (quality is than volume) PLA solution of 4-dioxane preparation.
2, add 22.5g NaCl, wherein the KCl diameter is between 100 microns～400 microns.
3, pour preset temperature under the stirring into and be quenching in-15 ℃ the mould.
4, after freezing 20 minutes, die sinking obtains the sample of desired shape.
5, in-15 ℃, lyophilize 4 days under 0.001325MPa～0MPa.
6, take out sample, it is immersed deionized water, changed water one time, soaked 3 days in per 8 hours.
7, vacuum-drying is 1 day, and temperature is 37 ℃, and pressure is 0.001325MPa～0MPa.
Tissue, organ porous holder for repairing are promptly made.
Claims (1)
1, a kind of particle that is separated leaches the method that legal system is organized fully, organ is used repair porous scaffold, it is characterized in that this method comprises following each step:
(1) biocompatible polymer is mixed with solution, polymkeric substance any in the multipolymer of multipolymer, poly(lactic acid), lactic acid and the oxyacetic acid of poly-(3-butyric ester), 3-butyric ester and 3-hydroxycaproic ester wherein, solvent is 1,4-dioxane or 1,4-dioxane: 1 of water=100: 0～15,4-dioxane-water mixture, the mass percent concentration that makes this solution is 5%～25%;
(2) get the pore former of particle diameter in 100 microns～400 micrometer ranges by the standard sieve sieve, pore former is NaCl, KCl;
(3) in the mass ratio of polymkeric substance and pore former be 1: 9～1: 30 ratio, the pore former in above-mentioned (2) is joined in the polymers soln in (1) step, stir;
(4) stir, the mixture in 3 is poured into quenching in the mould of preset temp, quench temperature is between-180 ℃～11.8 ℃, and quenching time is 5 minutes～2 hours;
(5) die sinking, in type goods lyophilize, freezing temp is between-130 ℃～11.8 ℃, and drying pressure is at 0.001325MPa～0MPa, sublimation drying two days～four days;
(6) goods with the lyophilize in (5) step are soaked into deionized water, change deionized water, and take out goods after 72 hours in per 8 hours;
(7) with the goods vacuum-drying in (6) step, temperature is 37 ℃, and pressure is 0.001325MPa～0MPa, dry 24 hours, is porous support of the present invention.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00105637A CN1095497C (en) | 2000-04-14 | 2000-04-14 | Method for preparation of repairing porous frame usedd for tissue and organ by a phase separation filter method |
| PCT/IB2001/000633 WO2001082988A1 (en) | 2000-04-14 | 2001-04-17 | Phase separated particle preparation method for a porous framework used in the prostheses of tissue and organs |
| AU2001246764A AU2001246764A1 (en) | 2000-04-14 | 2001-04-17 | Phase separated particle preparation method for a porous framework used in the prostheses of tissue and organs |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00105637A CN1095497C (en) | 2000-04-14 | 2000-04-14 | Method for preparation of repairing porous frame usedd for tissue and organ by a phase separation filter method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1275617A CN1275617A (en) | 2000-12-06 |
| CN1095497C true CN1095497C (en) | 2002-12-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00105637A Expired - Fee Related CN1095497C (en) | 2000-04-14 | 2000-04-14 | Method for preparation of repairing porous frame usedd for tissue and organ by a phase separation filter method |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN1095497C (en) |
| AU (1) | AU2001246764A1 (en) |
| WO (1) | WO2001082988A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431622C (en) * | 2005-12-08 | 2008-11-12 | 东南大学 | Method of organizing polymer porous support material for engineering and its preparation device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218109A (en) * | 1997-09-22 | 1999-06-02 | 任春严 | Production of organs for transplantation and method and apparatus for renovation and restoration |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5502092A (en) * | 1994-02-18 | 1996-03-26 | Minnesota Mining And Manufacturing Company | Biocompatible porous matrix of bioabsorbable material |
| US5686091A (en) * | 1994-03-28 | 1997-11-11 | The Johns Hopkins University School Of Medicine | Biodegradable foams for cell transplantation |
| DE69625822T2 (en) * | 1995-05-01 | 2003-06-05 | Samyang Corp | IMPLANTABLE, BIORESORBABLE MEMBRANE AND METHOD FOR THE PRODUCTION THEREOF |
| US6187329B1 (en) * | 1997-12-23 | 2001-02-13 | Board Of Regents Of The University Of Texas System | Variable permeability bone implants, methods for their preparation and use |
-
2000
- 2000-04-14 CN CN00105637A patent/CN1095497C/en not_active Expired - Fee Related
-
2001
- 2001-04-17 WO PCT/IB2001/000633 patent/WO2001082988A1/en active Application Filing
- 2001-04-17 AU AU2001246764A patent/AU2001246764A1/en not_active Abandoned
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218109A (en) * | 1997-09-22 | 1999-06-02 | 任春严 | Production of organs for transplantation and method and apparatus for renovation and restoration |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431622C (en) * | 2005-12-08 | 2008-11-12 | 东南大学 | Method of organizing polymer porous support material for engineering and its preparation device |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2001246764A1 (en) | 2001-11-12 |
| CN1275617A (en) | 2000-12-06 |
| WO2001082988A1 (en) | 2001-11-08 |
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Granted publication date: 20021204 |