CN105727364A - 一种纳微米多尺度聚乳酸三维支架及其制备方法 - Google Patents
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Abstract
本发明涉及一种纳微米多尺度聚乳酸三维支架及其制备方法，它采用在一定条件下分别静电纺丝纳米和微米壳聚糖纤维膜，按一定配比将纳米和微米壳聚糖纤维膜在水中高速剪切成短纤维，分样后，加入微米尺度的晶体碳酸钙颗粒作为致孔剂，经冷冻干燥成型，稀盐酸去除致孔剂，水洗后再经冷冻干燥得到纳微米多尺度聚乳酸三维支架。该制备方法工艺简单，纤维直径可控，孔径大小可控，支架在纤维直径和孔径同时具有微纳米尺度，赋予支架良好的综合性能。
Description
技术领域
本发明涉及一种纳微米多尺度聚乳酸三维支架及其制备方法，属于生物医用材料技术领域。
背景技术
聚乳酸作为美国FDA最早批准的一种合成聚合物支架材料，具有无毒、与人体相容性好、在体内可完全降解吸收等优点，被广泛地应用于骨、软骨、血管和皮肤等组织和器官的修复（LeeEJ等，AnnBiomedEng，2014;42(2):323）。支架的微观结构对其综合性能有较大的影响，研究表明纳米纤维支架有较大的比表面积和吸附位点，可增强蛋白质的吸附和细胞粘附和分化，从而可促进组织的再生。但单纯的纳米纤维力学强度较低，无法应用在力学强度要求较高的组织和器官的修复中。相比而言，微米纤维支架具有较好的力学性能，并且降解速率慢，能够维持支架植入过程中的结构稳定性。因此，在支架中同时具有纳米和微米纤维的微观结构则可以克服生物相容性和力学性能之间的矛盾。另外，支架要求具有三维贯通的孔结构，便于营养物质的传递、代谢物质的交换以及细胞的迁移。研究表明，对于营养物质的传递和代谢物质的交换，纳米尺度的孔具有较高的效率，并可促进支架的降解吸收和组织再生，但该尺度的孔比细胞要小一个数量级，细胞无法在支架内部渗透和迁移，微米尺度的孔则对细胞的渗透、迁移以及新血管和神经的长入是比较有利的。微纳米共存的孔结构可以保证细胞生长过程中营养物质的传递、细胞的迁移以及新血管和神经生长所需的空间。综上，在纤维直径和孔径同时具有微纳米多尺度的三维支架具有良好的生物相容性和力学性能。目前聚乳酸在制备三维支架的过程中多采用热致相分离的方法，采用四氢呋喃或二噁烷等溶剂可分别得到纳米和微米纤维状支架，但其纤维直径和孔径的控制较为困难，同时得到纳微米结构则更为困难（CN103159977A）。目前研究者通过静电纺丝的方法也可获得聚乳酸纤维薄膜，但通过静电纺丝法得到三维支架也是非常困难的。因此，如何制备纤维直径和孔径同时具有微纳米多尺度的三维聚乳酸支架是一个巨大的挑战。
发明内容
本发明的主要设想是采用静电纺丝的方法分别制备纳米和微米聚乳酸薄膜，按一定配比将纳米和微米聚乳酸纤维膜混合，并将聚乳酸薄膜高速剪切成短纤维，分样后，加入微米尺度的致孔剂，经冷冻干燥成型，水置换去除致孔剂，再经冷冻干燥得到三维纳微米纤维聚乳酸支架。
本发明中三维纳微米多尺度聚乳酸支架的制备方法具体如下所述。
(1)静电纺丝纳米聚乳酸纤维膜，配制聚乳酸10.0%的溶液，溶剂为氯仿和二噁烷的混合物，体积比为70:30，纺丝电压在20～25kV之间。
(2)静电纺丝微米聚乳酸纤维膜，配制聚乳酸20.0%的溶液，溶剂为氯仿和二噁烷的混合物，体积比为90:10，纺丝电压为12～15kV之间。
(3)分别称取定量的纳米和微米聚乳酸纤维膜，加入到定量的水中，在水中高速剪切成短纤维。
(4)分样至称量瓶中，加入筛分后具有一定粒度分布的晶体碳酸钙作为致孔剂，在-18℃下冷冻成型并冻干。
(5)冻干后的样品经稀盐酸去除致孔剂，水洗后再经冷冻干燥可获得聚乳酸纳微米多尺度的三维支架。
本发明制得的聚乳酸纳微米多尺度的三维支架为白色圆盘，其形状和高度可在分样中采用不同的容器和分样体积调节。纳微米多尺度的结构赋予支架良好的生物相容性和力学强度。该制备方法工艺简单，制备中也可方便地调整纺丝条件得到不同直径的纳米和微米聚乳酸纤维，相比于单纯的静电纺丝法，该法可容易地制备三维结构的支架。
具体实施方式
下面结合具体实施例，对本发明内容作进一步的说明，但本发明的实现方式并不局限于此。
实施例1：分别取7ml的氯仿和3ml的二噁烷，混合均匀，称取1.0g聚乳酸，搅拌溶解，静置12小时。将聚乳酸溶液加入到注射器中，通以20kV的电压纺丝，收集在接地的铝箔上，可获得聚乳酸纤维直径在50-750nm的薄膜。分别取9ml的氯仿和1ml的二噁烷，混合均匀，称取2.0g聚乳酸，搅拌溶解，静置12小时。将聚乳酸溶液加入到注射器中，通以15kV的电压纺丝，收集在接地的铝箔上，可获得聚乳酸纤维直径在1-10μm的薄膜。分别称取0.2g和0.8g纳米和微米聚乳酸纤维膜，在100ml水中高速剪切成短纤维，分样至称量瓶中，加入筛分的晶体碳酸钙颗粒，其粒度分布在50-350μm之间，高度与分样的液面相同，在-18℃下冷冻成型，在冻干机中冻干。冻干后的样品经稀盐酸去除支架中的致孔剂，水洗后再经冷冻干燥可获得聚乳酸纳微米多尺度的三维支架。
实施例2：分别取21ml的氯仿和9ml的二噁烷，混合均匀，称取3.0g聚乳酸，搅拌溶解，静置12小时。将聚乳酸溶液加入到注射器中，通以25kV的电压纺丝，收集在接地的铝箔上，可获得聚乳酸纤维直径在50-300nm的薄膜。分别取9ml的氯仿和1ml的二噁烷，混合均匀，称取2.0g聚乳酸，搅拌溶解，静置12小时。将聚乳酸溶液加入到注射器中，通以12kV的电压纺丝，收集在接地的铝箔上，可获得聚乳酸纤维直径在1-10μm的薄膜。分别称取2.4g和0.6g纳米和微米聚乳酸纤维膜，在100ml水中高速剪切成短纤维，分样至称量瓶中，加入筛分的晶体碳酸钙颗粒，其粒度分布在50-350μm之间，高度与分样的液面相同，在-18℃下冷冻成型，在冻干机中冻干。冻干后的样品经稀盐酸去除支架中的致孔剂，水洗后再经冷冻干燥可获得聚乳酸纳微米多尺度的三维支架。
Claims (6)
1.一种聚乳酸纳微米多尺度的三维支架及其制备方法，其特征在于在一定条件下分别静电纺丝纳米和微米聚乳酸纤维膜，按一定配比将纳米和微米聚乳酸纤维膜在水中高速剪切成短纤维，分样后，加入微米尺度的晶体碳酸钙颗粒作为致孔剂，经冷冻干燥成型，稀盐酸去除致孔剂，水洗后再经冷冻干燥得到纳微米多尺度聚乳酸三维支架。
2.根据权利要求1所述的聚乳酸纳微米多尺度的三维支架及其制备方法，其特征在于所使用的聚乳酸分子量在5～10万之间。
3.根据权利要求1所述的聚乳酸纳微米多尺度的三维支架及其制备方法，其特征在于静电纺丝纳米纤维膜时，聚乳酸浓度为10.0%，溶剂为氯仿和二噁烷的混合物，体积比为70:30，纺丝电压在20～25kV之间。
4.根据权利要求1所述的聚乳酸纳微米多尺度的三维支架及其制备方法，其特征在于静电纺丝微米聚乳酸纤维膜时，聚乳酸浓度为20.0%，溶剂为氯仿和二噁烷的混合物，体积比为90:10，纺丝电压在12～15kV之间。
5.根据权利要求1所述的聚乳酸纳微米多尺度的三维支架及其制备方法，其特征在于纳米聚乳酸和微米聚乳酸的质量比在20:80到80:20之间，聚乳酸纳米微米纤维在水中的总浓度在1～3%之间。
6.根据权利要求1所述的纳微米多尺度聚乳酸三维支架及其制备方法，其特征在于使用的晶体碳酸钙致孔剂的粒度范围在50～350μm之间。
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| CN108704165A (zh) * | 2017-12-15 | 2018-10-26 | 中国科学院深圳先进技术研究院 | 海藻酸盐复合浆料、海藻酸空心管及其制备方法 |
| WO2022148564A1 (de) * | 2021-01-08 | 2022-07-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Hochporöse nanofaservliese als trägerstruktur für stromales gewebe |
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| CN103285424A (zh) * | 2013-05-27 | 2013-09-11 | 东华大学 | 一种三维纤维基气凝胶组织工程支架及其制备方法 |
| WO2014160019A1 (en) * | 2013-03-14 | 2014-10-02 | Lifenet Health | Aligned fiber and method of use thereof |
| CN104888278A (zh) * | 2015-05-20 | 2015-09-09 | 东华大学 | 一种纳/微米纤维三维多孔结构支架材料及其制备和应用 |
| CN105107022A (zh) * | 2015-09-21 | 2015-12-02 | 东华大学 | 一种在湿态下具有压缩弹性的纳米纤维多孔支架的制备方法 |
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| CN103127553A (zh) * | 2013-03-05 | 2013-06-05 | 青岛大学 | 一种纳米微米结构共存壳聚糖双层支架的制备方法 |
| WO2014160019A1 (en) * | 2013-03-14 | 2014-10-02 | Lifenet Health | Aligned fiber and method of use thereof |
| CN103285424A (zh) * | 2013-05-27 | 2013-09-11 | 东华大学 | 一种三维纤维基气凝胶组织工程支架及其制备方法 |
| CN104888278A (zh) * | 2015-05-20 | 2015-09-09 | 东华大学 | 一种纳/微米纤维三维多孔结构支架材料及其制备和应用 |
| CN105107022A (zh) * | 2015-09-21 | 2015-12-02 | 东华大学 | 一种在湿态下具有压缩弹性的纳米纤维多孔支架的制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704165A (zh) * | 2017-12-15 | 2018-10-26 | 中国科学院深圳先进技术研究院 | 海藻酸盐复合浆料、海藻酸空心管及其制备方法 |
| WO2022148564A1 (de) * | 2021-01-08 | 2022-07-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Hochporöse nanofaservliese als trägerstruktur für stromales gewebe |
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| CN105727364B (zh) | 2018-08-03 |
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