CN116271221A - 一种抗菌抗氧化的复合纳米纤维支架及其制备方法 - Google Patents
一种抗菌抗氧化的复合纳米纤维支架及其制备方法 Download PDFInfo
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- CN116271221A CN116271221A CN202310235064.9A CN202310235064A CN116271221A CN 116271221 A CN116271221 A CN 116271221A CN 202310235064 A CN202310235064 A CN 202310235064A CN 116271221 A CN116271221 A CN 116271221A
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Abstract
本发明公开了一种抗菌抗氧化的复合纳米纤维支架及其制备方法，该支架为负载CuNPs@MBG‑THC纳米颗粒的聚己内酯/明胶静电纺丝支架。本发明利用铜纳米颗粒释放的铜离子抑制伤口处的细菌增殖，通过重要活性成分四氢姜黄素和介孔活性玻璃的释放，清除伤口处过量的ROS，并能有效促进成纤维细胞增殖，胶原沉积，细胞外基质积累和血管生成的，有利于伤口的快速愈合。
Description
技术领域
本发明涉及一种医用纳米纤维支架材料及其制备方法，尤其涉及一种抗菌抗氧化的复合纳米纤维支架及其制备方法。
背景技术
皮肤伤口愈合是一个复杂、协调和多方面的自然和动态的再生过程，通常包括止血、炎症、增殖和组织再生四个阶段。然而，对于感染性伤口，持续的细菌感染和炎症反应，通常会阻碍伤口的快速愈合。感染性伤口部位持续的炎症反应会产生过量的活性氧(ROS)和炎症因子，过量的ROS和炎症因子通过对细胞膜、DNA和蛋白质氧化损伤阻碍细胞增殖并导致细胞凋亡，促使伤口愈合长期停留在炎症期而不能有效愈合。因此，迫切需要开发一种抗菌能力和抗氧化能力强、生物相容性好的可降解伤口再生支架。
铜(Cu)是人体必需的微量元素，在大多数生物化学和生理过程中起重要作用。近年来，铜纳米粒子(CuNPs)因其广谱的抗菌活性、较低的毒性高效的催化能力而受到越来越多的关注。然而，CuNPs在空气中和溶剂中极不稳定，颗粒粒度分布广，容易氧化聚集，稳定性差，很难长久储存，并且体内过量释放出的铜离子对细胞也有一定的毒性，这也极大地阻碍了其临床应用。
四氢姜黄素(THC)是姜黄素的一种主要代谢物，具有和姜黄素几乎类似的生理和药理特性。研究表明，与姜黄素相比，THC具有更好的药理作用和临床优势，如有效的抗肿瘤活性，更强大的抗氧化，抗糖化，抗炎和抗衰老的作用，并能有效促进成纤维细胞，胶原沉积，细胞外基质积累和血管生成的，这些都是有效促进伤口愈合的因素。
生物活性玻璃(BG)具有良好的生物相容性，成骨和血管生成能力，是一种可用于临床的组织再生材料。已有文献报道，在纳米纤维，水凝胶，3D打印支架中加入BG可以显著提高支架的力学性能和成骨能力，促进新生骨和血管的再生。在众多BG中，介孔生物活性玻璃(MBG)因其粒径/孔大小结构可调，比表面积大，载药量大等优点，在皮肤伤口愈合应用中作为生物活性物质和药物载体受到越来越多的关注。
发明内容
发明目的：本发明的目的在于提供一种生物相容性好、同时具有促进皮肤组织愈合和抗氧化的双重功效的抗菌抗氧化的复合纳米纤维支架；
本发明的第二个目的在于提供上述抗菌抗氧化的复合纳米纤维支架的制备方法。
技术方案：本发明所述的抗菌抗氧化的复合纳米纤维支架，所述支架是负载了多功能介孔活性玻璃的聚己内酯/明胶静电纺丝纳米纤维膜。
其中，所述的多功能介孔活性玻璃为铜纳米颗粒封端的负载四氢姜黄素的介孔活性玻璃。
上述抗菌抗氧化的复合纳米纤维支架的制备方法，将聚己内酯、明胶和多功能介孔活性玻璃溶解于溶剂中，搅拌，利用静电纺丝得到复合纳米纤维膜。
其中，所述聚己内酯的分子量为8-20W；在这个范围内的更有利于聚己内酯静电纺丝；聚己内酯和明胶的质量比为1：4-5：5；所述的溶剂为六氟异丙醇，三氟乙醇，二氯甲烷，甲醇，N,N-二甲基甲酰胺中的一种或多种；所述静电纺丝溶液中的聚己内酯/明胶的质量浓度为10-20％；多功能介孔活性玻璃的质量浓度为0.3-3％。
其中，所述的多功能介孔活性玻璃通过以下方法制备得到：
(1)将二价铜盐溶液、稳定剂溶液搅拌混合，加入还原剂，在加热条件下反应至溶液为黄棕色，离心，取上清液进行透析，产物经冷冻干燥得到CuNPs粉末；
(2)将十六烷基三甲基溴化铵溶解于水中，调节pH值为8-11，向反应体系中间歇加入正硅酸四乙酯、多聚磷酸和乙酸钙，搅拌，离心，洗涤，产物经煅烧以去除十六烷基三甲基溴化铵，得到介孔活性玻璃粉末，记为MBG粉末；
(3)将MBG粉末溶解在含有四氢姜黄素的无水醇溶液中，搅拌，离心，洗涤；将沉淀分散于含有3-氨丙基三乙氧基硅烷的水中，在加热条件下搅拌，经离心洗涤，将沉淀重新分散于水中，得到氨基修饰的MBG-THC溶液；
(4)将步骤(1)所得的CuNPs粉末分散在柠檬酸溶液中，得到CuNPs-COOH溶液，将1-乙基-(3-二甲基氨基丙基)碳化二亚胺加入CuNPs-COOH溶液中，与步骤(3)得到的氨基修饰的MBG-THC溶液混合搅拌，得到终产物CuNPs@MBG-THC，离心，洗涤，冷冻干燥，制得。
其中，所述步骤(1)中，二价铜盐为氯化铜，硫酸铜，乙酸铜和硝酸铜中的一种；稳定剂为壳聚糖、BSA和聚乙烯吡咯烷酮中的至少一种；还原剂为抗坏血酸、硼氢化钠和硫酸亚铁中的至少一种。
其中，所述步骤(1)中，所述加热条件优选为在50-100℃的油浴锅中持续搅拌，搅拌反应时间为1-12h；离心所述转速为10000-20000rpm，离心时间为15-60min；透析的参数为：3500D的透析袋透析12-48h；得到的CuNPs粉末的粒径为3-5nm。
其中，所述步骤(2)中，加入正硅酸四乙酯的量为3-5mL；加入多聚磷酸的量为0.3-0.5mL；加入乙酸钙的量为1.5-3.6g。
其中，所述步骤(2)中，搅拌的时间为0.5-4h；煅烧的参数为：煅烧温度500-700℃，煅烧时间1-5h；可有效去除模板剂CTAB且不改变MBG本身结构。
其中，所述步骤(3)中，四氢姜黄素的浓度为0.5-2mg/mL；所述步骤(3)中，无水醇溶液中的MBG的浓度为0.5-2mg/mL；无水醇溶液优选为无水甲醇或无水乙醇；CuNPs-COOH溶液浓度为0.5-2mg/mL；最终得到的氨基修饰的MBG-THC溶液的浓度为0.5-4mg/mL；MBG粉末溶解在含有四氢姜黄素的无水乙醇中后，离心的转速为4000-9000rpm；有利于达到清洗颗粒而不对吸附的THC造成影响。
其中，所述步骤(3)中，在加热条件下搅拌的参数为：温度40-80℃，搅拌时间为8-24h；将沉淀分散于含有3-氨丙基三乙氧基硅烷的水中之后离心的转速为7000-9000rpm。
所述步骤(4)中，柠檬酸溶液的浓度为10-100mg/mL；CuNPs-COOH溶液浓度为0.5-2mg/mL；所述CuNPs-COOH溶液和氨基修饰的MBG-THC溶液的浓度比为1:1-1:4。
其中，所述静电纺丝的具体工艺参数为：纺丝电压为15-20kv；纺丝液流速为1.5-3.5mL/h；针尖到接收器的距离为10-20cm；滚筒接收器的转速为50-150rpm/min；环境温度为20-30℃；环境湿度为30-60％。
有益效果：本发明与现有技术相比，取得如下显著效果：该支架生物相容性好，能够抵抗伤口处的细菌侵蚀，同时介孔活性玻璃负载了THC，可以有效缓释THC，同时具有促进皮肤组织愈合和抗氧化的双重功效，通过抗菌协调抗氧化作用，显著提高支架的伤口愈合疗效。
附图说明
图1为本发明实施例1制备的MBG-THC和CuNPs@MBG-THC纳米颗粒透射电镜图；
图2为本发明实施例1制备的CuNPs，CuNPs-COOH，MBG，MBG-THC和CuNPs@MBG-THC纳米颗粒的Zeta电位图；
图3为本发明实施例1制备的纳米纤维膜PG和PG/CuNPs@MBG-THC的扫描电镜图；
图4为本发明实施例1制备的复合纳米纤维膜PG和PG/CuNPs@MBG-THC抗菌扫描电镜图；
图5为本发明实施例1制备的复合纳米纤维膜PG和PG/CuNPs@MBG-THC在体外清除过氧化氢的测试结果；
图6为本发明实施例1制备的复合纳米纤维膜PG和PG/CuNPs@MBG-THC细胞生物相容性的测试结果。
具体实施方式
下面对本发明作进一步详细描述。
实施例1
提供一种具有抗菌和抗氧化作用的复合纳米纤维支架的制备方法，包括以下步骤：
1、多功能介孔活性玻璃，即CuNPs@MBG-THC的制备包括如下步骤：
(1)将50mM醋酸铜与0.1g PVP溶解在20mL去离子水中搅拌混合，然后缓慢加入10mL 100mM抗坏血酸溶液，在50℃的油浴锅中持续搅拌12h,反应溶液变成棕色，20000rpm离心15min，取上清液，使用3500D的透析袋透析48小时后，冷冻干燥，得到CuNPs粉末。
(2)在40℃下，将1g十六烷基三甲基溴化铵，以下记为CTAB，溶解在50mL去离子水中，加入氨水调节pH值为9，每隔30min依次向反应体系中加入3mL TEOS、0.3mL PPA和1.5g乙酸钙，搅拌4h，8000rpm离心洗涤沉淀，50℃烘干过夜，700℃煅烧5h，去除CTAB，得到介孔活性玻璃粉末，以下记为MBG粉末。
(3)将步骤(2)中得到的MBG粉末溶解在含有2mg/mL THC的无水乙醇中搅拌过夜，4000rpm离心洗涤沉淀，将沉淀重新分散在含有0.5mL 3-氨丙基三乙氧基硅烷的50mL去离子水中，在40℃下磁力搅拌24h，9000rpm离心洗涤沉淀，重新分散在去离子水中，得到氨基修饰的MBG-THC溶液。
(4)将步骤(1)所得的CuNPs粉末分散在浓度为10mg/mL的柠檬酸溶液中，超声作用20min，得到0.5mg/mL的CuNPs-COOH溶液，将5mg的1-乙基-(3-二甲基氨基丙基)碳化二亚胺，以下记为EDC，加入10mL CuNPs-COOH溶液中，与步骤(3)得到的10mL 0.5mg/mL氨基修饰的MBG-THC溶液混合搅拌，得到终产物CuNPs@MBG-THC，9000rpm离心洗涤，冷冻干燥。所得纳米颗粒的形貌如图1所示，与MBG-THC颗粒相比，CuNPs@MBG-THC纳米颗粒粒径显著增大，表面粗糙，说明CuNPs成功的包覆在MBG-THC表面。图2显示的纳米颗粒的电位变化也证实了最终CuNPs@MBG-THC的成功合成。
2、抗菌抗氧化复合静电纺丝支架的制备
将0.2g分子量为20W的聚己内酯，以下记为PCL，和0.8g明胶，以下记为Gel，溶解于10mL六氟异丙醇中搅拌均匀得到质量分数为10％的聚己内酯/明胶溶液，以下记为PG溶液，2小时后加入3mg CuNPs@MBG-THC超声混匀，磁力搅拌过夜，进行静电纺丝，得到复合纳米纤维膜。从图3结果可知，与PG膜相比，加入CuNPs@MBG-THC的膜的纤维更粗，空隙更大。
静电纺丝的具体工艺参数为：纺丝电压为15kv；纺丝液流速为1.5mL/h；针尖到接收器的距离为10cm；滚筒接收器的转速为150rpm/min；环境温度为20℃；环境湿度为30％。
将一定浓度的大肠杆菌和金黄色葡萄球菌分别接种在PG和PG/CuNPs@MBG-THC膜表面培养24小时，利用扫描电镜观察细菌数量。结果如图4所示，其中，图4中的A、B为接种在PG膜表面的扫描电镜图，C、D为接种在PG/CuNPs@MBG-THC膜表面的扫描电镜图；且C、D分别为培养24小时后的扫描电镜图。可以看出，与PG相比，培养24小时后PG/CuNPs@MBG-THC膜上的细菌数量显著减少，证明CuNPs@MBG-THC的加入提高的膜的抗菌能力。
将膜与500μM的过氧化氢溶液在黑暗环境中孵育一定的时间，通过二甲酚橙法检测膜的清除过氧化氢的能力。如图5所示，随着时间的推移，PG膜没有显示出过氧化氢的清除能力，加入CuNPs@MBG-THC，能显著提升PG膜的过氧化氢清除能力。
利用CCK-8实验检测了膜的细胞毒性，如图6所示，加入CuNPs@MBG-THC的膜与PG膜相比，更能促进细胞的增殖且没有细胞毒性，证实了膜的生物安全性。
实施例2
提供一种具有抗菌和抗氧化作用的复合纳米纤维支架的制备方法，包括以下步骤：
1、多功能介孔活性玻璃的制备包括如下步骤：
(1)将50mM硫酸铜与0.1g壳聚糖溶解在20mL去离子水中搅拌混合，然后缓慢加入10mL 100mM硫酸亚铁溶液，在100℃的油浴锅中持续搅拌1h，反应溶液变成棕色，15000rpm离心30min，取上清液，使用3500D的透析袋透析12小时后，冷冻干燥，得到CuNPs粉末。
(2)在30℃下，将1g十六烷基三甲基溴化铵溶解在50mL去离子水中，加入氨水调节pH值为8，每隔30min依次向反应体系中加入4mL TEOS、0.4mL PPA和2.8g乙酸钙，搅拌0.5h，8000rpm离心洗涤沉淀，50℃烘干过夜，500℃煅烧1h，去除CTAB，得到介孔活性玻璃粉末。
(3)将步骤(2)中得到的MBG粉末溶解在含有1mg/mL THC的无水乙醇中搅拌过夜，6000rpm离心洗涤沉淀，将沉淀重新分散在含有1.5mL 3-氨丙基三乙氧基硅烷的50mL去离子水中，在60℃下磁力搅拌8h，9000rpm离心洗涤沉淀,重新分散在去离子水中，得到氨基修饰的MBG-THC溶液。
(4)将步骤(1)所得的CuNPs粉末分散在浓度为50mg/mL的柠檬酸溶液中，超声作用20min，得到1mg/mL的CuNPs-COOH溶液，将15mg的1-乙基-(3-二甲基氨基丙基)碳化二亚胺加入10mL CuNPs-COOH溶液中，与步骤(3)得到的10mL4mg/mL氨基修饰的MBG-THC溶液混合搅拌5min，得到终产物CuNPs@MBG-THC，9000rpm离心洗涤，冷冻干燥。
2、抗菌抗氧化复合静电纺丝支架的制备
将0.75g分子量为8W的聚己内酯和0.75g明胶溶解于10mL六氟异丙醇中搅拌均匀得到质量分数为15％的PG溶液，2小时后加入15mg CuNPs@MBG-THC超声混匀，磁力搅拌过夜，进行静电纺丝，得到复合纳米纤维膜。
静电纺丝的具体工艺参数为：纺丝电压为17kv；纺丝液流速为2mL/h；针尖到接收器的距离为18cm；滚筒接收器的转速为100rpm/min；环境温度为25℃；环境湿度为50％。
实施例3
提供一种具有抗菌和抗氧化作用的复合纳米纤维支架的制备方法，包括以下步骤：
1、多功能介孔活性玻璃的制备包括如下步骤：
(1)将50mM氯化铜与0.1g BSA溶解在20mL去离子水中搅拌混合，然后缓慢加入10mL100mM硼氢化钠溶液，在80℃的油浴锅中持续搅拌6h,反应溶液变成棕色，10000rpm离心60min，取上清液，使用3500D的透析袋透析24小时后，冷冻干燥，得到CuNPs粉末。
(2)在25℃下，将1g十六烷基三甲基溴化铵溶解在50mL去离子水中，加入氨水调节pH值为11，每隔30min依次向反应体系中加入5mL TEOS、0.5mL PPA和3.6g乙酸钙，搅拌2h，8000rpm离心洗涤沉淀，50℃烘干过夜，600℃煅烧3h，去除CTAB，得到介孔活性玻璃粉末。
(3)将步骤(2)中得到的MBG粉末溶解在含有0.5mg/mL THC的无水乙醇中搅拌过夜，9000rpm离心洗涤沉淀，将沉淀重新分散在含有1mL 3-氨丙基三乙氧基硅烷的50mL去离子水中，在80℃下磁力搅拌16h，9000rpm离心洗涤沉淀,重新分散在去离子水中，得到氨基修饰的MBG-THC溶液。
(4)将步骤(1)所得的CuNPs粉末分散在浓度为100mg/mL的柠檬酸溶液中，超声作用20min，得到2mg/mL的CuNPs-COOH溶液，将20mg的1-乙基-(3-二甲基氨基丙基)碳化二亚胺加入10mL CuNPs-COOH溶液中，与步骤(3)得到的10mL 3mg/mL氨基修饰的MBG-THC溶液混合搅拌，得到终产物CuNPs@MBG-THC，9000rpm离心洗涤，冷冻干燥。
2、抗菌抗氧化复合静电纺丝支架的制备
将0.5g分子量为12W的聚己内酯和1.5g明胶溶解于10mL六氟异丙醇中搅拌均匀得到质量分数为20％的PG溶液，2小时后加入60mg CuNPs@MBG-THC超声混匀，磁力搅拌过夜，进行静电纺丝，得到复合纳米纤维膜。
静电纺丝的具体工艺参数为：纺丝电压为20kv；纺丝液流速为3.5mL/h；针尖到接收器的距离为20cm；滚筒接收器的转速为50rpm/min；环境温度为30℃；环境湿度为60％。
对比例1
在实施例1的基础上，与实施例1不同的是制备铜纳米颗粒时没有加稳定剂，结果铜纳米颗粒粒径大，且分布不均匀。
对比例2
在实施例1的基础上，与实施例1不同的是制备介孔活性玻璃时溶液pH>11，结果为纳米颗粒粒径大于500纳米，孔径超过20纳米。
对比例3
在实施例1的基础上，与实施例1不同的是制备介孔活性玻璃是煅烧温度小于500℃，时间少于1h，结果CTAB没有完全去除。
对比例4
在实施例1的基础上，与实施例1不同的是制备的MBG-THC颗粒清洗时离心速度小于4000rpm，结果大量吸附在MBG表面的THC没有洗掉，影响实验结果。
对比例5
在实施例1的基础上，与实施例1不同的是PCL的分子量为6W，结果纺丝液由于粘度过低不能在接收器上成膜。
对比例6
在实施例1的基础上，与实施例1不同的是PCL：Gel＝1:9，结果不能在接受器上成膜。
Claims (10)
1.一种抗菌抗氧化的复合纳米纤维支架，其特征在于，所述支架是负载了多功能介孔活性玻璃的聚己内酯/明胶静电纺丝纳米纤维膜。
2.根据权利要求1所述的抗菌抗氧化的复合纳米纤维支架，其特征在于，所述的多功能介孔活性玻璃为铜纳米颗粒封端的负载四氢姜黄素的介孔活性玻璃。
3.一种权利要求1所述抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，将聚己内酯、明胶和多功能介孔活性玻璃溶解于溶剂中，搅拌，利用静电纺丝得到复合纳米纤维膜。
4.根据权利要求3所述抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述聚己内酯的分子量为8-20W；聚己内酯和明胶的质量比为1：4-5：5。
5.根据权利要求3所述抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述静电纺丝溶液中的聚己内酯/明胶的质量浓度为10-20％；多功能介孔活性玻璃的质量浓度为0.3-3％。
6.根据权利要求3所述的抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述的多功能介孔活性玻璃通过以下方法制备得到：
(1)将二价铜盐溶液、稳定剂溶液搅拌混合，加入还原剂，在加热条件下反应至溶液为黄棕色，离心，取上清液进行透析，产物经冷冻干燥得到CuNPs粉末；
(2)将十六烷基三甲基溴化铵溶解于水中，调节pH值为8-11，向反应体系中间歇加入正硅酸四乙酯、多聚磷酸和乙酸钙，搅拌，离心，洗涤，产物经煅烧以去除十六烷基三甲基溴化铵，得到介孔活性玻璃粉末，记为MBG粉末；
(3)将MBG粉末溶解在含有四氢姜黄素的无水醇溶液中，搅拌，离心，洗涤；将沉淀重新分散在含有3-氨丙基三乙氧基硅烷的水中，在加热条件下搅拌，离心，洗涤；将沉淀重新分散在水中，得到氨基修饰的MBG-THC溶液；
(4)将步骤(1)所得的CuNPs粉末分散在柠檬酸溶液中，得到CuNPs-COOH溶液，将1-乙基-(3-二甲基氨基丙基)碳化二亚胺加入CuNPs-COOH溶液中，与步骤(3)得到的氨基修饰的MBG-THC溶液混合搅拌，得到终产物CuNPs@MBG-THC，离心，洗涤，冷冻干燥，制得。
7.根据权利要求5所述的抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述步骤(3)中，MBG粉末溶解在含有四氢姜黄素的无水乙醇中后，离心的转速为4000-9000rpm。
8.根据权利要求5所述的抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述步骤(2)中，煅烧的温度为500-700℃，时间为1-5h。
9.根据权利要求5所述的抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述CuNPs-COOH溶液和氨基修饰的MBG-THC溶液的浓度比为1:1-1:4。
10.根据权利要求3所述的抗菌抗氧化的复合纳米纤维支架的制备方法，其特征在于，所述静电纺丝的具体工艺参数为：纺丝电压为15-20kv；纺丝液流速为1.5-3.5mL/h；针尖到接收器的距离为10-20cm；滚筒接收器的转速为50-150rpm/min。
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102242463A (zh) * | 2011-04-20 | 2011-11-16 | 东华大学 | 一种静电纺制备明胶/聚己内酯复合纳米纤维膜的方法 |
| CN105688274A (zh) * | 2016-01-20 | 2016-06-22 | 江苏省人民医院 | 一种聚己内酯/明胶电纺复合支架的制备工艺 |
| KR20160073811A (ko) * | 2014-12-17 | 2016-06-27 | 단국대학교 천안캠퍼스 산학협력단 | 생체활성 유리 나노스피어를 포함하는 섬유 스캐폴드, 이의 제조방법, 및 이의 용도 |
| US20180117215A1 (en) * | 2017-10-11 | 2018-05-03 | Maryam Eslami | Scaffold for skin tissue engineering and a method of synthesizing thereof |
| WO2018090925A1 (zh) * | 2016-11-16 | 2018-05-24 | 华南理工大学 | 一种皮肤烧伤修复材料及其制备方法 |
| CN108478843A (zh) * | 2018-02-06 | 2018-09-04 | 中国科学院金属研究所 | 具有含铜涂层的医用敷料及其制备方法 |
| CN113289059A (zh) * | 2021-06-02 | 2021-08-24 | 江西理工大学 | 一种含铜介孔生物玻璃-镁金属复合抗菌材料及其制备方法和应用 |
| CN114855365A (zh) * | 2022-04-12 | 2022-08-05 | 华南理工大学 | 一种载药金属有机骨架复合静电纺丝纤维膜及其制备方法与应用 |
-
2023
- 2023-03-13 CN CN202310235064.9A patent/CN116271221A/zh active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102242463A (zh) * | 2011-04-20 | 2011-11-16 | 东华大学 | 一种静电纺制备明胶/聚己内酯复合纳米纤维膜的方法 |
| KR20160073811A (ko) * | 2014-12-17 | 2016-06-27 | 단국대학교 천안캠퍼스 산학협력단 | 생체활성 유리 나노스피어를 포함하는 섬유 스캐폴드, 이의 제조방법, 및 이의 용도 |
| CN105688274A (zh) * | 2016-01-20 | 2016-06-22 | 江苏省人民医院 | 一种聚己内酯/明胶电纺复合支架的制备工艺 |
| WO2018090925A1 (zh) * | 2016-11-16 | 2018-05-24 | 华南理工大学 | 一种皮肤烧伤修复材料及其制备方法 |
| US20180117215A1 (en) * | 2017-10-11 | 2018-05-03 | Maryam Eslami | Scaffold for skin tissue engineering and a method of synthesizing thereof |
| CN108478843A (zh) * | 2018-02-06 | 2018-09-04 | 中国科学院金属研究所 | 具有含铜涂层的医用敷料及其制备方法 |
| CN113289059A (zh) * | 2021-06-02 | 2021-08-24 | 江西理工大学 | 一种含铜介孔生物玻璃-镁金属复合抗菌材料及其制备方法和应用 |
| CN114855365A (zh) * | 2022-04-12 | 2022-08-05 | 华南理工大学 | 一种载药金属有机骨架复合静电纺丝纤维膜及其制备方法与应用 |
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