CN101781815B - Preparation method of porous fiber with controllable degradation rate for tissue engineering scaffold - Google Patents
Preparation method of porous fiber with controllable degradation rate for tissue engineering scaffold Download PDFInfo
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- CN101781815B CN101781815B CN 201010104863 CN201010104863A CN101781815B CN 101781815 B CN101781815 B CN 101781815B CN 201010104863 CN201010104863 CN 201010104863 CN 201010104863 A CN201010104863 A CN 201010104863A CN 101781815 B CN101781815 B CN 101781815B
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Abstract
The invention relates to a preparation method of porous fiber with a controllable degradation rate for a tissue engineering scaffold, which comprises the following steps: uniformly mixing a biodegradable polymer and a pore-forming agent, vacuum drying, melt spinning, drawing, immersing into hydrochloric acid or distilled water to remove the pore-forming agent, and vacuum drying, thereby obtaining the porous fiber with micro pores with the diameters of 10-100mum uniformly distributed on the surface thereof. The preparation method of the invention is simple and is applicable to industrial production. The diameters of the micro pores of the prepared fiber are matched with cell sizes, so that cells can be easily adhered into the micro pores on the surface of the fiber for growth. Simultaneously, the degradation rate is controllable.
Description
Technical field
The invention belongs to the preparation field of porous fibre, particularly relate to the preparation method of the controlled porous fibre of a kind of degradation rate for tissue engineering scaffold.
Background technology
Up to now, be achieved the polyester material that is mainly of clinical practice in field of biomedical polymer materials, as polyglycolic acid (PGA), polycaprolactone (PCL), PLA (PLA), PPDO (PDO) etc.Therefore, aliphatic polyester has obtained using more and more widely in the field such as embedded material and organizational project in vivo.In order to control the biodegradability of aliphatic polyester, can be by changing that polymer architecture forms and form prepare the new bio medical macromolecular materials of different biodegradation rates, can significantly improve the physical and chemical performances such as the degraded of aliphatic polymer and thermodynamics.So far go back the single biomaterial of neither one and can satisfy organizational project to all demands of timbering material, this will comprehensively have the advantage of biomaterial now, it is organically merged, just can prepare and have biocompatibility, can transmitting tissue cell grow up, can supporting tissue in the tissue engineering bracket of growth and the performance such as assurance vivo degradation speed is controlled.
The degradation time of PGA, PLA, PDO was respectively 60 days, 220 days and 182 days, the degradation time of PGA is very fast, this has a great impact its application, regulate its degradation speed by molecular weight and molecular weight distribution significant limitation is arranged, therefore change degree of crystallinity and the hydrophily of PGA by the method for blend or copolymerization, thereby reach the purpose of controlling PGA class composite degradation speed.In addition, because the degradation cycle of block copolymer occupy between each polymer, also can come the control degradation behavior by regulating the ratio that each block becomes minute.Li S.M. philosophy has been done systematic research to the copolymer of PLA and PGA, PCL and the vivo degradation character of homopolymers, and discovery can be regulated degradation speed by the ratio of regulating lactide (LA), glycolide (GA) and caprolactone (CL).【LiSM，VertM.The?Encyclopedia?of?Controlled?DrugDelivery.Mathiowitz?E.ed，John?Wiley?&?Sons，New?York，1999】。With GA and LA copolymerization, by regulating the charge ratio of LA and GA, can the degraded character of PLGA be regulated and controled.The degradation time of PGLA (LA/GA=10/90,25/75,50/50,75/25) is respectively 90,100,120,180.
Aspect blend, PLA affects its biocompatibility and degradation property owing to having hydrophobicity, therefore study more.In PLA complete biodegradable co-mixing system, PLA by with the blend such as poly 3-hydroxy butyrate (PHB), PCL, polyoxyethylene (PEO), starch, can change mechanical performance, processing characteristics and the degradation speed of composite.But have no the report about PGA and PLA or PDO blended complex.
Composite support of tissue engineering can also become fibrage certain shape and structure to use except simple use biodegradable fiber, and the standby support of fibrage legal system is commonly used in the aspects such as tendon, cartilage, blood vessel and neural reparation of organizational project.Jin Yiming etc. adopt the PDO fiber through compiling the blood vessel support arm, and result shows that the PDO supporting structure stablize and has a compression reaction performance preferably, and the external degradation test shows degradation rate that its maintenance within 8 weeks is comparatively stable and mechanical property preferably.[Jin Yiming, Wang Wenzu. the external degradation performance of warp knit structure blood vessel support arm. Chinese Tissue Engineering Study and clinical rehabilitation, 2008,12 (27): 5248-5252].The biodegradable fiber fabric of single component can not satisfy tissue repair usually to the requirement of mechanics support and degradation time, the Wu Shuan congruence adopts PLA, 4 kinds of weaving threads of polyglycolic acid long filament braiding preparation of different component ratio, discovery is in degradation process, increase along with PGA fibre composition ratio in weaving thread, the degradation speed of weaving thread is also constantly accelerated, the weaving thread mass loss rate increases, and brute force reduces gradually.[Wu Shuanquan, Zhang Peihua, Guo are just. the external degradation performance of different proportion PGA/PLA weaving thread. and Donghua University's journal (natural science edition), 2009,35 (3): 274-303].Yuan Xiaoyan etc. have openly invented a kind of preparation method of multi-component hybridized 3 D woven myotendinous rack material, respectively contain a certain proportion of copolymer aliphatic poly ester fiber as material take PGA, polylactide or they, be woven into column-braid shape rope dress 3 D weaving tendon stent material with 1 * 1 four circular 3 D weaving method of step, have advantages of that tensile strength is good, degradation speed can regulate and control, cellular affinity is good.[Yuan Xiaoyan etc. the preparation method of multi-component hybridized 3 D woven myotendinous rack material (CN 1194774C)].
Porous fibre has the structure by using some traditional phase disengagement methods to make.These methods generally include mixes fluoropolymer resin with diluent or plasticizer, polymer solution is carried out coolingly being separated to cause in a kind of liquid medium, stays a kind of crosslinked loose structure thereby then rinse out diluent; Add a certain amount of inorganic particulate spinning technique in the spinning melt of polyester, stretch and remove inorganic particulate by the alkali decrement, stay micropore at fiber surface, utilize the capillarity of micropore, can improve the hygroscopicity of fiber and obtain nice and cool feel.
A kind of micropore polyester fibre, it is characterized in that being formed by conventional resin and water-soluble modified polymer resin, in 70～50%: 30～50% even blend of ratio, and dissolve 8～12% water-soluble modified polymer resin after melt spinning, its surface and innerly be evenly distributed with the micropore that a large amount of diameters are about 0.5～2 μ m aperture.[Qian Jianhua etc. a kind of micropore polyester fibre and preparation method (CN 101144206A)].A kind of microcellular foamed fiber, when forming that polymer that fiber uses melts and when mixing in extruder, supercritical fluid is introduced extruder, then the unidirectional solution of melt and gas is extruded the formation micropore by the spinning head of filament spinning component, the micropore L/D ratio greater than 1, filament diameter is greater than 5 μ m, micro-pore diameter is less than 10 μ m.[Cui Rong hundred etc. microcellular foamed fiber and preparation method thereof (CN 1304652C)].Poplar grace is peaceful to be waited take calcium carbonate as pore former, is drawn into doughnut by mixing mutually with polypropylene, carries out post processing with hydrochloric acid, just forms porous after being mixed in the calcium carbonate stripping in doughnut.[Yang Enning, Guo Jing .CaCO
3The research of/polypropene blended preparation porous polypropylene fibre. synthetic fiber, 2006,2:25-27].
Present domestic PGA, PLA, single polymer of PDO or the mixing of copolymer or polymer of employing that not yet have prepares tissue engineering bracket porous fibre and fabric.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the controlled porous fibre of a kind of degradation rate for tissue engineering scaffold, and the method is simple, and cost is low, is suitable for suitability for industrialized production; Micro-pore diameter and the cell size of gained fiber are complementary, and make cell be easy to adhere to growth in the micropore of fiber surface, and degradation rate is controlled simultaneously.
The preparation method of the porous fibre that a kind of degradation rate for tissue engineering scaffold of the present invention is controlled comprises:
Be evenly to mix at 90～99%: 1～10% by weight percentage with biodegradable polymer and pore former, vacuumize 21-48h, carry out melt spinning, stretch, immerse afterwards in hydrochloric acid or distilled water, remove pore former, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 10～100 μ m micropores.
Described biodegradable polymer is the mixing of two or three in single polymer of polyglycolic acid PGA, polylactic acid PLA, PPDO PDO.
Described biodegradable polymer is the copolymer of polyglycolic acid PGA, polylactic acid PLA or PPDO PDO.
Described biodegradable polymer is the mixing of two or three in the polymer of polyglycolic acid PGA, polylactic acid PLA, PPDO PDO.
The molecular weight of described PGA is 10～150,000, and the molecular weight of PLA is 10～150,000, and the molecular weight of PDO is 10～150,000.
Described biodegradable polymer is the PGLA of the mass ratio 1～99/99～1 of GA/LA.
Described pore former is calcium carbonate or polyvinylpyrrolidone (PVP) particle, and particle diameter is 10～80 μ m.
The concentration of described hydrochloric acid is 6%.
Described porous fibre obtains the porous fibre fabric through braiding, and weaving manner is same fibrage or different proportion fiber interweaving.
The porous fibre fabric is wire, tubulose or plane form.
The present invention is different according to the object that organizational project is repaired, and selects PGA, the PLA of Different Weight ratio and PDO fiber to carry out shuffling, and the degradation time of fibrous framework and the speed of growth of cell are complementary, and promotes the reparation of tissue.
Organizational project cell and support composite demand timbering material and cell have good compatibility, can be conducive to the attaching growth of cell on support.Generally, the fiber surface for preparing by melt spinning is dense smooth, in order to improve the adherent situation of cell on biodegradable fiber, can prepare the micropore that is consistent with cell size at fiber surface, cell can be dropped in these micropores, be difficult for peeling off support, can strengthen the degree of roughness of fiber surface simultaneously, improve the compatibility of cell and timbering material.
the diameter range of cell is 10～100 μ m, in order to prepare the micropore of this pore diameter range on fiber surface, method with water-soluble polymer-modified resin stripping is too small with the micro-pore diameter that the method for introducing the supercritical fluid drilling obtains, cell is dropped in micropore, and the size in wayward aperture, therefore select the particle of known diameter as pore former, by preparing fiber with the degradable polymer blend, last stripping pore former prepares the micropore of certain diameter, this method is simple, can be to environment, and cost of material is low, good reproducibility.
Beneficial effect
(1) preparation method of the present invention is simple, and cost is low, is suitable for suitability for industrialized production;
(2) micro-pore diameter of gained fiber of the present invention and cell size are complementary, make cell be easy to adhere to growth in the micropore of fiber surface, degradation rate is controlled simultaneously, the mechanical property decay rate of material and the Healing Rate of tissue are complementary, be conducive to the compound cultivation of organizational project cell and support, can be as tissue engineering cell scaffolds such as nerve or blood vessels.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Be 100,000 PGA with molecular weight, molecular weight is that pore former calcium carbonate that section (mass ratio of GA/LA is 75/25) and the particle diameter of 100,000 PLA is 50 μ m is that the ratio of 95%: 5% is evenly mixed by weight percentage, melt spinning is carried out in vacuumize after 24 hours, stretch, the fiber immersion concentration that then will prepare gained is to remove pore former in 6% hydrochloric acid, changed a hydrochloric acid solution in every 6 hours during this time, take out fiber after 24 hours, obtaining the surface uniform distribution after vacuumize and diameter is arranged is the porous fibre of 50～60 μ m micropores.
Embodiment 2
Be 120,000 PGA with molecular weight, molecular weight is that pore former calcium carbonate that section (mass ratio of GA/LA is 90/10) and the particle diameter of 120,000 PLA is 20 μ m is that the ratio of 98%: 2% is evenly mixed by weight percentage, melt spinning is carried out in vacuumize after 24 hours, stretch, the fiber immersion concentration that then will prepare gained is to remove pore former in 6% hydrochloric acid, changed a hydrochloric acid solution in every 6 hours during this time, take out fiber after 24 hours, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 20～35 μ m micropores.
Embodiment 3
Be 100,000 PGA with molecular weight, molecular weight is that pore former PVP percentage by weight that section (PGA is 50/50 with the weight ratio of PDO) and the particle diameter of 100,000 PDO is 80 μ m is that the ratio of 99%: 1% is evenly mixed, melt spinning is carried out in vacuumize after 24 hours, stretch, the fiber that then will prepare gained immerses in distilled water removes pore former, changed first water in every 6 hours during this time, take out fiber after 24 hours, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 80～100 μ m micropores.
Embodiment 4
Be that the ratio of 93%: 7% is evenly mixed with the section of PGLA (the GA/LA mass ratio is 75/25) and the particle diameter pore former PVP percentage by weight that is 10 μ m, melt spinning is carried out in vacuumize after 24 hours, stretch, the fiber that then will prepare gained immerses in distilled water removes pore former, changed first water in every 6 hours during this time, take out fiber after 24 hours, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 10～15 μ m micropores.
Embodiment 5
Be 100,000 PGA with molecular weight, molecular weight is that the section of 100,000 PLA is that the ratio of 98%: 2% is evenly mixed with the particle diameter pore former PVP percentage by weight that is 10 μ m respectively, melt spinning is carried out in vacuumize after 24 hours, stretch, the fiber that then will prepare gained immerses in distilled water removes pore former, changed first water in every 6 hours during this time, and took out fiber after 24 hours, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 10～15 μ m micropores.Choose 4 PGA porous long filaments and 2 PLA porous long filaments weave on the 6 vertical spindle braiding machines of ingot, change gear 30 teeth, 54.5 °, weaving angle, make the weaving thread of 4PGA/2PLA, the diameter 0.18mm of this weaving thread, ultimate strength 1276.2cN, coefficient of friction 0.72.
Embodiment 6
Be 150,000 PGA with molecular weight, molecular weight is that the section of 150,000 PLA is that the ratio of 98%: 2% is evenly mixed with the particle diameter pore former PVP percentage by weight that is 10 μ m respectively, melt spinning is carried out in vacuumize after 24 hours, stretch, the fiber that then will prepare gained immerses in distilled water removes pore former, changed first water in every 6 hours during this time, and took out fiber after 24 hours, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 10～15 μ m micropores.Choose 2 PGA porous long filaments and 4 PLA porous long filaments weave on the 6 vertical spindle braiding machines of ingot, change gear 30 teeth, 54.5 °, weaving angle, make the weaving thread of 2PGA/4PLA, the diameter 0.22mm of this weaving thread, ultimate strength 1061.1cN, coefficient of friction 0.72.
Claims (3)
1. the preparation method of the controlled porous fibre of a degradation rate for tissue engineering scaffold, it is characterized in that: concrete steps are as follows:
Be that 90～99%:1～10% evenly mixes by weight percentage with biodegradable polymer and pore former, vacuumize 21-48h, carry out melt spinning, stretch, immerse afterwards in hydrochloric acid or distilled water, remove pore former, obtain surface uniform after vacuumize and be distributed with the porous fibre that diameter is 10～100 μ m micropores;
Wherein, pore former is calcium carbonate or polyvinylpyrrolidone PVP, and particle diameter is 10～80 μ m;
Biodegradable polymer is the mixing of two or three in single polymer of polyglycolic acid PGA, polylactic acid PLA, PPDO PDO; The copolymer of polyglycolic acid PGA, polylactic acid PLA or PPDO PDO; The mixing of two or three in the polymer of polyglycolic acid PGA, polylactic acid PLA, PPDO PDO; The molecular weight of PGA is 10～150,000, and the molecular weight of PLA is 10～150,000, and the molecular weight of PDO is 10～150,000.
2. the preparation method of the controlled porous fibre of a kind of degradation rate for tissue engineering scaffold according to claim 1, it is characterized in that: described biodegradable polymer is the PGLA of the mass ratio 1～99/99～1 of GA/LA.
3. the preparation method of the controlled porous fibre of a kind of degradation rate for tissue engineering scaffold according to claim 1, it is characterized in that: the concentration of described hydrochloric acid is 6%.
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