CN110331579A - 一种抗菌的表面功能化苯胺低聚体纳米纤维及其制备方法和应用 - Google Patents

一种抗菌的表面功能化苯胺低聚体纳米纤维及其制备方法和应用 Download PDF

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CN110331579A
CN110331579A CN201910544876.5A CN201910544876A CN110331579A CN 110331579 A CN110331579 A CN 110331579A CN 201910544876 A CN201910544876 A CN 201910544876A CN 110331579 A CN110331579 A CN 110331579A
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闵永刚
刘荣涛
王勇
刘屹东
廖松义
张诗洋
庞贻宇
肖天华
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Guangdong University of Technology
Dongguan South China Design and Innovation Institute
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Abstract

本发明公开了一种抗菌的表面功能化苯胺低聚体纳米纤维及其制备方法和应用。该功能化苯胺低聚体纳米纤维是在氮气或氩气的惰性气氛下，将苯胺低聚体加入到有机溶剂中完全溶解，加入溶于相同有机溶液的可降解高分子搅拌均匀，在30～80℃下加入催化剂进行反应，经过滤、洗涤、干燥得到苯胺低聚体‑可降解高分子复合材料；将该复合材料溶于有机溶剂，静电纺丝后得到苯胺低聚体纳米纤维；将得到的纳米纤维表面处理后浸泡在含有抗菌药物的相同有机溶液中，洗涤、干燥后得到。本发明中表面功能化苯胺低聚体纳米纤维在外界电磁场环境下，能够促进细胞粘附、增殖和分化、具有生物降解性能、生物相容性好、制备方法简单、合成简单、副产物少特点。

Description

一种抗菌的表面功能化苯胺低聚体纳米纤维及其制备方法和 应用
技术领域
本发明属于载药和组织工程生物医用领域，更具体地，涉及一种抗菌的表面功能化苯胺低聚体纳米纤维及其制备方法和应用。
背景技术
大分子量的聚苯胺具有良好的生物相容性，在外界电磁场作用下可促进细胞分化、增值和生长，但其溶解性较差，体液环境下不易排出体外。然而低聚体苯胺在生物相容性和掺杂状态下的导电性与聚苯胺相差无几，但其溶解性大大提高。可降解高分子材料具有极好的生物相容性，在体液环境下可逐步分解为可吸收或排出的小分子而引起重视，在医用材料领域也得到了进一步的发展。因此，合成一种基于低聚体苯胺的可降解并具有抗菌性的复合纳米纤维作为生物支架材料在载药和组织工程生物医用领域具有巨大的潜力。
发明内容
为了解决上述现有技术存在的不足和缺点，本发明目的在于提供一种抗菌的表面功能化苯胺低聚体纳米纤维。
本发明的另一目的在于提供上述抗菌的表面功能化苯胺低聚体纳米纤维的制备方法。
本发明的再一目的在于提供一种上述抗菌的表面功能化苯胺低聚体纳米纤维的应用。
本发明的目的通过下述技术方案来实现：
一种抗菌的表面功能化苯胺低聚体纳米纤维，所述的苯胺低聚体纳米纤维是在保护气氛下，将苯胺低聚体加入到有机溶剂中完全溶解，加入溶于相同有机溶液的可降解高分子搅拌均匀，在30～80℃下加入催化剂进行反应，经过滤、洗涤、干燥得到苯胺低聚体-可降解高分子复合材料；将该复合材料溶于有机溶剂，静电纺丝后得到苯胺低聚体纳米纤维；将得到的纳米纤维表面处理后浸泡在含有抗菌药物的相同有机溶液中，经洗涤、干燥后得到。
优选地，所述的苯胺低聚体为苯胺三聚体、苯胺四聚体、苯胺五聚体、苯胺六聚体、苯胺七聚体或苯胺八聚体。
优选地，所述的有机溶剂为乙醇、乙醚、丙酮、二氯甲烷、氯仿、二硫化碳、甲苯、四氢呋喃、N,N-二甲基甲酰胺、苯甲酸或N-甲基吡咯烷酮中的一种以上。
优选地，所述的抗菌药物为青霉素、氨基糖苷类、喹诺酮类、姜黄素、阿霉素、硫酸软骨素、肝素、硫酸乙酰肝素、硫酸皮肤素或硫酸用层素的一种以上。
优选地，所述的可降解高分子为聚己内酯、聚乳酸、聚羟基乙酸、聚乳酸-羟基乙酸共聚物、聚乙二醇或上述材料的衍生物；所述的催化剂为脂肪酶或辛酸亚锡。
优选地，所述的苯胺低聚体和可降解高分子的质量比为1：(1～9)；所述催化剂为苯胺低聚体质量的0.1～10wt％；所述的含有抗菌药物在有机溶液中的质量浓度为5～50wt％。
优选地，所述的表面处理采用等离子束溅射沉积法、紫外辐射法、物理气相沉积法或磁控溅射法。
优选地，所述的保护气氛为氮气或氩气；所述反应的时间为4～50h。
所述的抗菌的表面功能化苯胺低聚体纳米纤维的制备方法，包括如下具体步骤：
S1.在保护气氛下，将苯胺低聚体加入到有机溶剂中完全溶解，加入溶于相同有机溶液的可降解高分子搅拌均匀，在30～80℃下加入催化剂进行反应，经过滤、洗涤、干燥得到苯胺低聚体-可降解高分子复合材料；
S2.将上述复合材料溶于相同有机溶剂，静电纺丝后得到苯胺低聚体纳米纤维；
S3.将得到的纳米纤维表面处理后浸泡在含有抗菌药物的相同有机溶液中，经洗涤、干燥后得到抗菌的表面功能化苯胺低聚体纳米纤维。
所述的抗菌的表面功能化苯胺低聚体纳米纤维在生物组织工程支架材料领域中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明中抗菌的低聚体苯胺表面功能化纳米纤维具有良好的抗菌性、生物相容性和可降解性；
2.本发明的表面功能化苯胺低聚体纳米纤维在外界电磁环境下可影响此纳米纤维材料的降解，促进细胞在现为上的黏附、增值和分化；
3.本发明制备方法简单，合成条件温和，副产物少。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。
实施例1
1.在氮气气氛下，将8g苯胺三聚体溶于100mlDMF中完全溶解，向其中加入50ml已充分溶剂8gPCL的DMF混合液，搅拌均匀。
2.在30℃下加入0.1g脂肪酶反应15h，搅拌转速为300r/min，反应完成后用去离子水冲洗干净，50℃真空干燥箱处理12h后得到苯胺三聚体-PCL复合材料。
3.5g复合材料溶于DMF中，静电纺丝得到纳米纤维后40℃真空干燥8h，紫外辐射后，浸入到30％的姜黄素DMF溶液中得到含有姜黄素的苯胺三聚体-PCL纳米纤维。
将得到含有姜黄素的苯胺三聚体-PCL纳米纤维用于培养成骨细胞，其表面接触角为118.5°，表面润湿性良好，在10mV电场作用下，成骨细胞密度较空白组增加25％，培养7d后，支架材料质量损失量为40％，姜黄素仍有72.5％的释放潜力。
实施例2
1.氩气气氛下，将5g苯胺四聚体溶于50ml二氯甲烷中完全溶解，向其中加入30ml已充分溶剂5gPEG的二氯甲烷混合液，搅拌均匀。
2.在50℃下加入0.05g脂肪酶反应20h，搅拌转速为250r/min，反应完成后用去离子水冲洗干净，60℃真空干燥箱处理10h后得到苯胺四聚体-PCL复合材料。
3.4g复合材料溶于二氯甲烷中，静电纺丝得到纳米纤维后50℃真空干燥12h，等离子体溅射表面处理后浸入到50％的阿霉素二氯甲烷溶液含有阿霉素的苯胺四聚体-PEG纳米纤维。
将得到含有阿霉素的苯胺四聚体-PEG纳米纤维用于培养成骨细胞，其表面接触角为107.2°，表面润湿性良好，在100Hz磁场作用下，成骨细胞密度较空白组增加32.4％，培养14d后，支架材料质量损失量为55.6％，阿霉素仍有42.5％的释放潜力。
实施例3
1.氮气气氛下，将1g苯胺八聚体溶于100mlN-甲基吡咯烷酮中完全溶解，向其中加入50ml已充分溶剂9gPLA的N-甲基吡咯烷酮混合液，搅拌均匀。
2.在60℃下加入0.05g脂肪酶反应40h，搅拌转速为250r/min，反应完成后用去离子水冲洗干净，60℃真空干燥箱处理10h后得到苯胺四聚体-PLA复合材料。
3.4g复合材料溶于二氯甲烷中，静电纺丝得到纳米纤维后50℃真空干燥12h，等离子体溅射表面处理后浸入到含有60％肝素的N-甲基吡咯烷酮溶液中，得到苯胺八聚体-PLA纳米纤维。
将得到含有阿霉素的苯胺八聚体-PLA纳米纤维用于培养成骨细胞，其表面接触角为121.8°，表面润湿性良好，在150Hz磁场作用下，成骨细胞密度较空白组增加40.6％，培养30d后，支架材料质量损失量为35.2％，肝素仍有32.8％的释放潜力。
实施例4
1.氮气气氛下，将2g苯胺五聚体溶于50ml氯仿中完全溶解，向其中加入50ml已充分溶剂6gPGA的氯仿混合液，搅拌均匀。
2.在80℃下加入0.1g脂肪酶反应24h，搅拌转速为250r/min，反应完成后用去离子水冲洗干净，50℃真空干燥箱处理12h后得到苯胺五聚体-PGA复合材料。
3.4g复合材料溶于氯仿中，静电纺丝得到纳米纤维后50℃真空干燥12h，磁控溅射表面处理后浸入到含有40％硫酸用层素的氯仿溶液中，得到苯胺五聚体-PGA纳米纤维。
将得到含有阿霉素的苯胺五聚体-PGA纳米纤维用于培养成骨细胞，其表面接触角为117.3°，表面润湿性良好，在10Mv、100Hz电磁场作用下，成骨细胞密度较空白组增加35.7％，培养60d后，支架材料质量损失量为75.2％，硫酸用层素仍有16.9％的释放潜力。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

1.一种抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的苯胺低聚体纳米纤维是在保护气氛下，将苯胺低聚体加入到有机溶剂中完全溶解，加入溶于相同有机溶液的可降解高分子搅拌均匀，在30～80℃下加入催化剂进行反应，经过滤、洗涤、干燥得到苯胺低聚体-可降解高分子复合材料；将该复合材料溶于有机溶剂，静电纺丝后得到苯胺低聚体纳米纤维；将得到的纳米纤维表面处理后浸泡在含有抗菌药物的相同有机溶液中，经洗涤、干燥后得到。
2.根据权利要求1所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的苯胺低聚体为苯胺三聚体、苯胺四聚体、苯胺五聚体、苯胺六聚体、苯胺七聚体或苯胺八聚体。
3.根据权利要求1所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的有机溶剂为乙醇、乙醚、丙酮、二氯甲烷、氯仿、二硫化碳、甲苯、四氢呋喃、N,N-二甲基甲酰胺、苯甲酸或N-甲基吡咯烷酮中的一种以上。
4.根据权利要求1所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的抗菌药物为青霉素、氨基糖苷类、喹诺酮类、姜黄素、阿霉素、硫酸软骨素、肝素、硫酸乙酰肝素、硫酸皮肤素或硫酸用层素的一种以上。
5.根据权利1要求所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的可降解高分子为聚己内酯、聚乳酸、聚羟基乙酸、聚乳酸-羟基乙酸共聚物、聚乙二醇或上述材料的衍生物；所述的催化剂为脂肪酶或辛酸亚锡。
6.根据权利要求1所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的苯胺低聚体和可降解高分子的质量比为1：(1～9)；所述催化剂为苯胺低聚体质量的0.1～10wt％；所述的含有抗菌药物在有机溶液中的质量浓度为5～50wt％。
7.根据权利要求1所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的表面处理采用等离子束溅射沉积法、紫外辐射法、物理气相沉积法或磁控溅射法。
8.根据权利要求1所述的抗菌的表面功能化苯胺低聚体纳米纤维，其特征在于，所述的保护气氛为氮气或氩气；所述反应的时间为4～50h。
9.根据权利要求1-8任一项所述的抗菌的表面功能化苯胺低聚体纳米纤维的制备方法，其特征在于，包括如下具体步骤：
S1.在保护气氛下，将苯胺低聚体加入到有机溶剂中完全溶解，加入溶于相同有机溶液的可降解高分子搅拌均匀，在30～80℃下加入催化剂进行反应，经过滤、洗涤、干燥得到苯胺低聚体-可降解高分子复合材料；
S2.将上述复合材料溶于相同有机溶剂，静电纺丝后得到苯胺低聚体纳米纤维；
S3.将得到的纳米纤维表面处理后浸泡在含有抗菌药物的相同有机溶液中，经洗涤、干燥后得到抗菌的表面功能化苯胺低聚体纳米纤维。
10.权利要求1-8任一项所述的抗菌的表面功能化苯胺低聚体纳米纤维在生物组织工程支架材料领域中的应用。
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