CN113491791A - 一种负载肝素的微纳复合纤维膜及其制备方法 - Google Patents

一种负载肝素的微纳复合纤维膜及其制备方法 Download PDF

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CN113491791A
CN113491791A CN202010252517.5A CN202010252517A CN113491791A CN 113491791 A CN113491791 A CN 113491791A CN 202010252517 A CN202010252517 A CN 202010252517A CN 113491791 A CN113491791 A CN 113491791A
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pcl
pvp
heparin
fiber membrane
micro
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张兴光
王威
王杰
郭丁丁
陈星�
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Suzhou Hexiang Textile Technology Co ltd
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Abstract

本申请涉及一种微纳复合纤维膜及其制备方法。本发明首次通过溶液喷纺技术制备得到了负载肝素的PCL/PVP复合微纳纤维膜，其具有表面光滑、直径均一、高生物活性等优点，该复合膜同时具备PCL/PVP复合膜良好的亲水性、可生物降解性等性能，又具有了胶原优异的生物活性，更兼具肝素抗凝血性、抗炎、抗过敏的功效，生物相容性和生物可降解性性能优良，可用于骨组织工程或作为生物体支架材料，便于大批量生产，具有良好的应用前景。

Description

一种负载肝素的微纳复合纤维膜及其制备方法
技术领域
本申请属于生物医用材料制备领域，涉及一种负载肝素的微纳复合纤维膜，尤其涉及一种采用溶液喷纺技术制备的负载肝素的微纳复合纤维膜。
背景技术
胶原具有良好的生物相容性、良好的保湿亲水性和可降解性、较好的诱导细胞粘附、分化与繁殖的作用，加之它是天然的高分子材料，在生物医用材料领域得到了广泛的应用，但胶原本身的强度较低，且不具有水溶性，而聚乙烯醇和聚乙烯吡咯烷酮是另一类长期使用的生物医用材料，其具有可纺性好、水溶性好、强度高等优点。将聚乙烯醇和聚乙烯吡咯烷酮与胶原进行共混，可以在一定程度上弥补胶原强度不足的缺点。肝素具有抗凝血性、抗炎、抗过敏的作用，可增强抗凝血酶3与凝血酶的亲和力，加速凝血酶的失活，抑制血小板的粘附聚集，增强蛋白c的活性，刺激血管内皮细胞释放抗凝物质和纤溶物质。还具有抑制血小板，增加血管壁的通透性，可调控血管新生以及调血脂的作用，在临床上应用广泛。
溶液喷纺技术是一种新型的制备微纳米纤维的方法，相较于传统的静电纺丝法，其无需电场环境，不需要高压设备或任何导电收集器，设备更加简单，可以更高的注射速度进行纺丝，易于操作，成本低廉，纺丝效率更高。聚合物的选择范围更加宽泛，不仅限于具有较高介电常数的聚合物，且采用的溶剂易于挥发且无毒性，更加绿色环保。溶液喷纺技术是通过将聚合物溶于挥发性溶剂中，并利用高速流动的加压气体处理聚合物溶液，以促进溶剂的挥发和纤维的沉积细化，从而将纤维沉积于基板或承载物表面。其制备得到的微纳米纤维具有较广的商业价值，如应用于聚合物增强物、医学治疗、PM2.5的过滤、电学和光学器件等。
本发明以简单、快速而高效的溶液喷纺技术制备微纳纤维，充分利用胶原的生物学性能和聚乙烯醇的力学性能，达到优势互补的效果，以期所得材料可被广泛用于生物医用材料、传感器材料、过滤材料、生物仿生等领域。
发明内容
为解决上述诸如问题，特经过潜心研究提出如下技术方案。
一种采用溶液喷纺技术制备的微纳复合纤维膜，其特征在于：该纳米纤维材料是由聚己内酯PCL、聚乙烯吡咯烷酮PVP、I型胶原和肝素为原料，通过溶液喷纺技术制备得到负载肝素的PCL/PVP复合微纳纤维膜，其中，肝素的浓度为5～20mg/ml，按重量份，PCL：PVP＝1～10：10～1，所述I型胶原采用胶原的醋酸溶液，其浓度为0.2～0.6wt％，所述纤维直径为10nm～0.8μm，纤维比表面积为150～185m2/g，微纳复合纤维膜的细胞毒性反应不大于1级。
优选地，肝素的浓度为8～17mg/ml，按重量份，PCL：PVP＝2～7：8～3。
优选地，所述纤维直径为50～690nm，纤维比表面积为160～175m2/g。
优选地，I型胶原的醋酸溶液浓度为0.5wt％。
一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其包括如下步骤：
(1)按重量份PCL：PVP＝1～10：10～1的比例称取聚己内酯PCL、聚乙烯吡咯烷酮PVP，并进行真空干燥，将PCL和PVP加入到有机溶剂中，于45℃超声搅拌至混合均匀，再加入浓度为5～20mg/ml的肝素和浓度为0.2～0.6wt％的I型胶原醋酸溶液，超声搅拌得到均匀分散液，即为聚合物喷纺原液；所述有机溶剂为二氯甲烷、乙醇、乙酸乙酯、丙酮中的任一种；
(2)将步骤(1)配置得到的聚合物喷纺原液经计量泵进行计量并进入喷丝头，随着聚合物喷纺原液从喷丝孔挤出并形成细流，同时采用喷射装置对细流进行高速气流吹射并拉伸，得到沉积于基板上的PCL/PVP的复合微纳纤维膜，其中，气流压力为50-80psi；
(3)将步骤(2)制备得到的纳米纤维膜在无菌洁净工作台上晾干，并采用剂量为10～20KGy/h60Co所产生的γ射线进行消毒灭菌处理，成型包装，即得负载肝素的PCL/PVP的复合微纳纤维膜。
优选地，肝素的浓度为8～17mg/ml，按重量份，PCL：PVP＝2～7：8～3，I型胶原的醋酸溶液浓度为0.5wt％。
优选地，步骤(1)中气流压力为70psi。
优选地，所述纤维直径为50～690nm，纤维比表面积为160～175m2/g。
有益效果
本发明提供的技术方案带来的有益效果是：本发明首次通过溶液喷纺技术制备得到了负载肝素的PCL/PVP复合微纳纤维膜，其具有表面光滑、直径均一、高生物活性等优点，PCL和PVP这两种聚合物因溶解度的不同在溶液喷纺过程中发生相分离的现象，通过溶液喷纺技术制备得到的纳米纤维膜表面及内部能够形成纳米级尺寸的通孔，且通孔相互贯通形成了网络结构，进一步增加纳米纤维的比表面积，利于细胞长入、生长和增殖，肝素具有抗凝血性、抗炎、抗过敏的作用，的优良特性，根据协同理论，复合膜同时具备了PCL/PVP复合膜良好的亲水性、可生物降解性等性能，又具有了胶原优异的生物活性，更兼具肝素抗凝血性、抗炎、抗过敏的作用，等功效，生物相容性和生物可降解性性能优良，可用于骨组织工程或作为生物体支架材料，功能多样，便于大批量生产，具有良好的应用前景。
具体实施方式
实施例1
一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其包括如下步骤：
(1)按重量份PCL：PVP＝5：8的比例称取聚己内酯PCL、聚乙烯吡咯烷酮PVP，并进行真空干燥，将PCL和PVP加入到二氯甲烷与乙醇的混合有机溶剂中，于45℃超声搅拌至混合均匀，再加入浓度为15mg/ml的肝素和浓度为0.4wt％的I型胶原醋酸溶液，超声搅拌得到均匀分散液，即为聚合物喷纺原液。
(2)将步骤(1)配置得到的聚合物喷纺原液经计量泵进行计量并进入喷丝头，随着聚合物喷纺原液从喷丝孔挤出并形成细流，同时采用喷射装置对细流进行高速气流吹射并拉伸，得到沉积于基板上的PCL/PVP的复合微纳纤维膜，其中，气流压力为60psi；
(3)将步骤(2)制备得到的纳米纤维膜在无菌洁净工作台上晾干，并采用剂量为15KGy/h60Co所产生的γ射线进行消毒灭菌处理，成型包装，即得负载肝素的PCL/PVP的复合微纳纤维膜。其纤维直径为453nm，纤维比表面积为165m2/g。
实施例2
一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其包括如下步骤：
(1)按重量份PCL：PVP＝2：5的比例称取聚己内酯PCL、聚乙烯吡咯烷酮PVP，并进行真空干燥，将PCL和PVP加入到二氯甲烷与乙醇的混合有机溶剂中，于45℃超声搅拌至混合均匀，再加入浓度为18mg/ml的肝素和浓度为0.5wt％的I型胶原醋酸溶液，超声搅拌得到均匀分散液，即为聚合物喷纺原液。
(2)将步骤(1)配置得到的聚合物喷纺原液经计量泵进行计量并进入喷丝头，随着聚合物喷纺原液从喷丝孔挤出并形成细流，同时采用喷射装置对细流进行高速气流吹射并拉伸，得到沉积于基板上的PCL/PVP的复合微纳纤维膜，其中，气流压力为70psi；
(3)将步骤(2)制备得到的纳米纤维膜在无菌洁净工作台上晾干，并采用剂量为15KGy/h60Co所产生的γ射线进行消毒灭菌处理，成型包装，即得负载肝素的PCL/PVP的复合微纳纤维膜。其纤维直径为120nm，纤维比表面积为158m2/g。
实施例3
一种过滤重金属离子的纳米纤维材料的制备方法，其包括如下步骤：
一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其包括如下步骤：
(1)按重量份PCL：PVP＝8：6的比例称取聚己内酯PCL、聚乙烯吡咯烷酮PVP，并进行真空干燥，将PCL和PVP加入到二氯甲烷与乙醇的混合有机溶剂中，于45℃超声搅拌至混合均匀，再加入浓度为18mg/ml的肝素和浓度为0.5wt％的I型胶原醋酸溶液，超声搅拌得到均匀分散液，即为聚合物喷纺原液。
(2)将步骤(1)配置得到的聚合物喷纺原液经计量泵进行计量并进入喷丝头，随着聚合物喷纺原液从喷丝孔挤出并形成细流，同时采用喷射装置对细流进行高速气流吹射并拉伸，得到沉积于基板上的PCL/PVP的复合微纳纤维膜，其中，气流压力为75psi；
(3)将步骤(2)制备得到的纳米纤维膜在无菌洁净工作台上晾干，并采用剂量为20KGy/h60Co所产生的γ射线进行消毒灭菌处理，成型包装，即得负载肝素的PCL/PVP的复合微纳纤维膜。其纤维直径为673nm，纤维比表面积为179m2/g。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (8)

1.一种采用溶液喷纺技术制备的微纳复合纤维膜，其特征在于：该纳米纤维材料是由聚己内酯PCL、聚乙烯吡咯烷酮PVP、I型胶原和肝素为原料，通过溶液喷纺技术制备得到负载肝素的PCL/PVP的复合微纳纤维膜，其中，肝素的浓度为5～20mg/ml，按重量份，PCL：PVP＝1～10：10～1，所述I型胶原采用胶原的醋酸溶液，其浓度为0.2～0.6wt％，所述纤维直径为10nm～0.8μm，纤维比表面积为150～185m2/g，微纳复合纤维膜的细胞毒性反应不大于1级。
2.根据权利要求1所述的一种采用溶液喷纺技术制备的微纳复合纤维膜，其特征在于，肝素的浓度为8～17mg/ml，按重量份，PCL：PVP＝2～7：8～3。
3.根据权利要求1-2所述的一种采用溶液喷纺技术制备的微纳复合纤维膜，其特征在于，所述纤维直径为50～690nm，纤维比表面积为160～175m2/g。
4.根据权利要求1-3所述的一种采用溶液喷纺技术制备的微纳复合纤维膜，其特征在于，I型胶原的醋酸溶液浓度为0.5wt％。
5.一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其包括如下步骤：
(1)按重量份PCL：PVP＝1～10：10～1的比例称取聚己内酯PCL、聚乙烯吡咯烷酮PVP，并进行真空干燥，将PCL和PVP加入到有机溶剂中，于45℃超声搅拌至混合均匀，再加入浓度为5～20mg/ml的肝素和浓度为0.2～0.6wt％的I型胶原醋酸溶液，超声搅拌得到均匀分散液，即为聚合物喷纺原液；所述有机溶剂为二氯甲烷、乙醇、乙酸乙酯、丙酮中的任一种；
(2)将步骤(1)配置得到的聚合物喷纺原液经计量泵进行计量并进入喷丝头，随着聚合物喷纺原液从喷丝孔挤出并形成细流，同时采用喷射装置对细流进行高速气流吹射并拉伸，得到沉积于基板上的PCL/PVP的复合微纳纤维膜，其中，气流压力为50-80psi；
(3)将步骤(2)制备得到的纳米纤维膜在无菌洁净工作台上晾干，并采用剂量为10～20KGy/h60Co所产生的γ射线进行消毒灭菌处理，成型包装，即得负载肝素的PCL/PVP的复合微纳纤维膜。
6.根据权利要求5所述的一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其特征在于，肝素的浓度为8～17mg/ml，按重量份，PCL：PVP＝2～7：8～3，I型胶原的醋酸溶液浓度为0.5wt％。
7.根据权利要求5所述的一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其特征在于，步骤(1)中气流压力为70psi。
8.根据权利要求5所述的一种负载肝素的PCL/PVP复合微纳纤维膜的制备方法，其特征在于，所述纤维直径为50～690nm，纤维比表面积为160～175m2/g。
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