CN115337441B - 一种枸杞提取物和纳米氧化锌纳米纤维膜的制备方法 - Google Patents
一种枸杞提取物和纳米氧化锌纳米纤维膜的制备方法 Download PDFInfo
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- CN115337441B CN115337441B CN202210814551.6A CN202210814551A CN115337441B CN 115337441 B CN115337441 B CN 115337441B CN 202210814551 A CN202210814551 A CN 202210814551A CN 115337441 B CN115337441 B CN 115337441B
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- nanofiber membrane
- zinc oxide
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- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
本发明涉及伤口敷料领域,提供了一种枸杞提取物和纳米氧化锌纳米纤维膜的制备方法,该纤维膜的基质材料为聚己内酯(PCL),负载物包括枸杞乙醇提取物和氧化锌纳米颗粒;纳米纤维膜通过静电纺丝得到。本发明中,采用静电纺丝得到负载有LBE和nZnO双重载药能力的纳米纤维膜,其中LBE起到良好的抗氧化作用,nZnO提高了纳米纤维膜的抗菌效果,实现纳米纤维膜抗氧化性能和抗菌功能的叠加。本发明将LBE和nZnO与PCL混合纺丝,制备方法简单,得到的纳米纤维膜具有良好的亲水、透湿、抗氧化、抗菌、生物相容性等优点。
Description
技术领域
本发明涉及一种含枸杞提取物和纳米氧化锌纳米纤维膜的制备方法,属于纳米纤维膜伤口敷料技术领域。
背景技术
伤口愈合过程复杂,涉及炎症反应、细胞增殖、迁移和分化,在伤口重塑过程中,许多细胞会产生氧自由基。过量的自由基会引起氧化应激反应,从而导致细胞、组织损伤,延迟伤口愈合,增加患者的痛苦。因此,通过抗氧化剂降低自由基水平可以减少氧化应激损伤,促进伤口愈合。
枸杞是茄科植物枸杞的成熟干果,一种传统的药食同源的植物,富含多糖、类黄酮、生物碱、维生素等活性成分。研究发现枸杞提取物(LBE)具有较强的抗氧化活性,能有效清除DPPH、ABTS等自由基,并且能显著降低大鼠骨骼肌细胞引起的氧化损伤。LBE还具有良好的抗炎活性,慢性伤口无法长期治愈的主要原因是炎症反应的反复发作,因此LBE是一种潜在的促进伤口愈合物质。
伤口愈合延迟的另一个主要原因是细菌感染。纳米氧化锌(nZnO)具有很强的抗菌作用,并且对革兰氏阳性菌和革兰氏阴性菌均具有明显的抑制作用。同时,低浓度nZnO对细胞没有副作用,可以被细胞正常代谢。因此,纳米氧化锌常被用作医用敷料中的抗菌剂。
静电纺丝是一种特殊的纤维制造工艺。利用该技术制备的纳米纤维膜在结构上类似于细胞外基质(ECM),可以为细胞提供支持和引导,有利于新组织的生长。同时,高比表面积和多孔结构能有效吸收伤口渗出物,维持伤口湿润的微环境,有利于载药。因此,已被广泛应用于生物医学敷料领域。目前,nZnO已被广泛用于抗菌医用敷料的制备,并提供了良好的抗菌抑菌效果,例如,专利号为CN202110502166.3的专利“一种抗菌作用的医用薄膜材料及其制备方法和应用”,专利号为CN202110912392.9的专利“一种纳米氧化锌/胶原基抗菌敷料及其制备方法”,专利号为CN201510301459.X的专利“一种具有抗菌抑菌功能的细菌纤维素敷料及其制备方法与应用”。但是利用LBE制备医用敷料鲜有报道,通过静电纺丝技术制备含有LBE的伤口敷料并结合nZnO良好的抗菌活性,有望制备出具有抗菌抗氧化作用的新型伤口敷料。
发明内容
本发明提供了一种含LBE和纳米氧化锌纳米纤维膜的制备方法,通过静电纺丝技术将LBE与nZnO结合制备出的纤维直径达到纳米级别,所形成的纳米纤维膜具有良好力学、润湿、透气、抗氧化、抗菌等性能,在伤口敷料方面表现出潜在的应用价值。
一种含LBE和纳米氧化锌纳米纤维膜,所述纳米纤维膜是以PCL作为基体,与LBE和nZnO混合制备纺丝前驱液进行静电纺丝所得。
本发明所述LBE的制备方法为:在水浴条件下对枸杞粉末进行乙醇回流提取,抽滤合并滤液,上清液经过真空旋转蒸发至一定体积,用等量的石油醚萃取三次,静置,取下层溶液继续旋转蒸发至干,即得到LBE。
优选地,称取50g粉碎均匀的枸杞粉末,加入400mL 80%乙醇溶液,在75℃的水浴条件下对枸杞粉末进行回流提取3次(2h/次),抽滤合并滤液,上清液经过真空旋转蒸发至20-35mL,用等量的石油醚萃取三次,静置,取下层溶液继续旋转蒸发至膏状,即得到LBE。
一种含LBE和纳米氧化锌纳米纤维膜的制备方法,包括如下步骤:
将PCL溶解在HFIP溶剂中,得到PCL溶液。
称取nZnO加入步骤A制备所得的溶液中均匀分散。
向步骤B所制备得分散液中添加LBE,磁力搅拌溶解得到纺丝前驱液。
将步骤C制备的纺丝前驱液进行静电纺丝,得到含有LBE和nZnO得纳米纤维膜。
优选地,所述含LBE和nZnO纳米纤维膜的制备方法如下,将基体材料PCL溶解于有机溶剂中,并将nZnO和LBE均匀分散在该溶液中,制备出纺丝前驱液,最后将纺丝溶液加入注射器中,通过静电纺丝装置进行高压静电纺丝,得到含LBE和nZnO的纳米纤维膜。
优选地,所述PCL的分子量为80000,HFIP为分析纯。
优选地,所述PCL的质量体积浓度为12-16%(w/v)。
优选地,所述nZnO的粒径大小≤20nm。
优选地,所述nZnO的添加量为2wt%,LBE的添加量为2.5-10%(w/v)。
优选地,所述步骤A、C搅拌时间为12h。
优选地,所述步骤B中超声功率为50W,超声时间为20min,超声3次。
所述静电纺丝的步骤具体为:将纺丝液加入注射器中,固定在静电纺丝微量注射泵上,调节纺丝参数进行静电纺丝,从而获得静电纺丝纤维膜。
优选地,静电纺丝装置可采用本领域内通用的技术手段和设备,注射器选用20mL,针头选用平头针头。
优选地,所述静电纺丝条件为:电压18—22KV、针尖到到滚筒的收集距离15—20cm、纺丝速度0.5-1mL/h、针头内径0.7-0.9mm、温度25-30℃、相对湿度小于30%。
所述制备方法获得的纳米纤维膜,其特征为:纤维直径为纳米级别,直径为324.67±117.9nm。
所述制备方法制备的含LBE和nZnO的纳米纤维膜在促进伤口敷料中的应用。
所述制备方法制备的含LBE和nZnO的纳米纤维膜,其特征为LBE有效成分为多糖类和黄酮类,有助于减少因伤口表面自由基过多所带来的氧化应激损伤和促进细胞增殖;nZnO有助于减少伤口表面的细菌感染,促进愈合。
本发明具有如下特点:
(1)本发明采用PCL作为纺丝基体材料,具有良好的生物降解性生物相容性,能与皮肤伤口直接接触,保证了安全无毒。
(2)本发明采用静电纺丝的形式制备的纳米纤维,一种能够高效、低成本制备纳米纤维的加工方式,能够仿生细胞外基质(ECM),在伤口修复过程中为细胞提供一定的支撑和引导,有利于上皮细胞的粘附、增殖、迁移和分化。
(3)本发明制备的PCL纤维直径在纳米级别,纤维直径达到188.61±44.98nm,利与LBE和nZnO的负载。(4)本发明所制备的含LBE和nZnO纳米纤维膜,具有良好的润湿性能,能有效吸收创面渗出液,并为伤口提供湿润的愈合环境。
(5)本发明所制备的含LBE和nZnO纳米纤维膜,具有良好的力学性能,能满足医用伤口敷料的力学性能需求。
(6)本发明所制备的含LBE和nZnO纳米纤维膜,具有适宜水蒸气透过性能,在保持伤口湿润环境的同时,有利与气体渗透和细胞呼吸。
(7)本发明所制备的含LBE和nZnO纳米纤维膜,具有明显的抗氧化效果,能减少因伤口表面自由过量所引起的氧化应激损伤。
(8)本发明所制备的含LBE和nZnO的纳米纤维膜具有抑菌性能,对金金黄色葡萄球菌(S.aureus)和大肠杆菌(E.coli)具有抑菌性能。
(9)本发明制备方法简单,对载体材料PCL电纺的同时,实现LBE和nZnO的双重负载效果,同时也扩宽枸杞在医用领域的应用。
附图说明:
图1为实施案例1PCL纳米纤维膜微观图和纤维直径分布直方图。
图2为实施案例2负载有nZnO的PCL纳米纤维膜微观图和纤维直径分布直方图。
图3为实施案例3负载有10%的LBE和氧化锌的纳米纤维膜微观图和纤维直径分布直方图。
图4为纳米纤维膜的接触角,其中(a)分别为案例3、4、5、6所述负载不同浓度的LBE纤维膜在3s、6s、9s和12s处的接触角,(b)(c)分别为纳米纤维膜和含nZnO纳米纤维膜的接触角。
图5为案例1、2、3、4、5、6所述纳米纤维膜的水蒸气透过率柱形图。
图6为案例1、2、3、4、5、6所述纳米纤维膜的力学性能表格。
图7为案例1、2、3、4、5、6所述纳米纤维膜的DPPH自由基清除率柱形图。
图8为案例1、2、3、4、5、6所述纳米纤维膜对S.aureus和E.coli的抑菌实验的抑菌圈图。
图9为案例1、2、3、4、5、6所述纳米纤维膜小鼠成纤维细胞(L929)的细胞增殖。
具体实施方式:
本发明所述制备的含LBE和nZnO纳米纤维膜的性能测试:
(1)水接触角测试
将纳米纤维膜裁剪2cm×3cm的条形,平铺在样品台上,使用移液枪在膜表面滴加3μL蒸馏水,分别记录3s、6s、9s、12s时每个纳米纤维膜的水接触角大小。
(2)水蒸气透过性测试
通过称重法评价纳米纤维膜对水蒸气的透过性能,将各组纳米纤维膜剪裁成一定的圆形,固定在瓶口直径40mm、含水量为30mL的瓶口上,并称重记录为Wi,置于在37℃、相对湿度为35%的环境中培养,24h后将瓶子取出,称重记录为Wf。水蒸气透过率(WVTR)由以下公式得到:
其中A是瓶口面积,Wi为初始重量,Wf为最终重量。
(3)力学性能测试
利用织物强度仪测量纳米纤维膜的拉伸断裂强度。将每组纳米纤维膜从锡箔纸上取下,分别切割成条带状(30×5mm),使用测厚仪测出每组纳米纤维膜的厚度,并以10mm/min的拉伸速度进行拉伸实验。每个样品测试5次。断裂强度由以下公式计算得到:
其中σb为样品的断裂强度,P为样品的最大断裂强度,S为样品的横截面积。
(4)抗氧化性能测试
精确称取50mg不同载药浓度纳米纤维膜,分别浸入5mL乙醇中,并置于100r/min、37℃的摇床中5h。然后取0.5mL浸出液加入2mL的DPPH溶液中,在黑暗中保持30min。用紫外分光光度计测量混合溶液在517nm处的吸光度,对照组用同等浓度的LBE溶液。自由基清除率有已下公式计算得到:
其中Ai为样品反应体系的吸光度,Aj为对照反应体系的吸光度,Ac为空白反应的吸光度。
(5)抗菌性能测试
将不同载药浓度的纳米纤维膜剪切成直径为8mm的圆片,紫外灭菌处理后,平贴在已接种细菌的培养基表面并轻轻按压,置于37℃的恒温培养箱中孵育15-24h后用游标卡尺测量每组纳米纤维膜的抑菌圈大小。
(6)细胞毒性测试
通过CCK-8法评价各组纳米纤维膜的细胞毒性,将各组纳米纤维膜(20mg),紫外杀菌处理后,并将其浸泡在2mL细胞培养液中24h。将小鼠成纤维细胞(L929)的细胞悬浮液(100μL)接种到96孔板中,并在37℃、5%CO2的环境中培养至孔底覆盖单层细胞,然后加入纳米纤维膜浸出液继续分别培养24和48h,向每个孔中添加10μL CCK-8,培养4h,用酶标仪测量每个孔的光密度值。
通过对所述纳米纳米纤维膜的接触角、透湿、抗氧化、抗菌和细胞毒性测试,评估了含LBE和氧化锌纳米纤维膜用于伤口敷料的潜能。
以下实施方案中所述LBE制备方法如下:
精确称取50g粉碎均匀的枸杞粉末,加入400mL 80%乙醇溶液,在75℃的水域条件下对枸杞粉末进行回流提取3次(2h/次),抽滤合并滤液,上清液经过真空旋转蒸发至一定体积,用等量的石油醚萃取3次,静置,取下层溶液继续旋转蒸发至干,即得到LBE。
实施案例1:
(1)精确称取1.5gPCL固体颗粒,加入10mL的六氟异丙醇(HFIP)溶液,置于磁力搅拌器上,室温条件搅拌12h使PCL充分溶解,配成浓度为15%(w/v)的纺丝液。
(2)将上述纺丝液倒入10mL带有平口针头的注射器中,通过纺丝装置进行高压静电纺丝,静电纺丝参数设置为:电压20KV、供料速度为0.6mL/h、接收距离为18cm、纺丝环境温度为30℃、纺丝时间为12h,通过滚筒接收器将纳米纤维膜收集到锡箔纸上,得到纯纺PCL纳米纤维膜。
(3)将纯纺PCL纳米纤维膜置于通风橱中,放置两周挥干表面残留溶剂,得到干燥的PCL纳米纤维膜。
(4)按上述方法制备的PCL纳米纤维膜,其表面形貌如图1所示,可以看出纤维表面光滑,随机取向,通过image J软件统计分析可知PCL纳米纤维平均直径达到188.61±44.98nm,并且纤维直径分布均匀。
实施案例2:
(1)精确称取1.5gPCL固体颗粒,加入10mL的HFIP溶液,置于磁力搅拌器上,室温条件搅拌12h使PCL充分溶解,配成浓度为15%(w/v)的纺丝液。
(2)在上述纺丝液中加入nZnO粉末,并置于磁力搅拌器上室温搅拌12h,然后将置于超声清洗机中进行超声20min,超声3次,获得含有nZnO的PCL纺丝液。
(3)将上述含有nZnO的纺丝液转移至10mL的带有平口针头的注射器中,通过纺丝装置进行高压静电纺丝,静电纺丝参数设置为:电压20KV、供料速度为0.6mL/h、接收距离为18cm、纺丝环境温度为30℃、纺丝时间为12h,通过滚筒接收器将纳米纤维膜收集到锡箔纸上,得到负载有nZnO的PCL纳米纤维膜。
(4)将上述所制备的纳米纤维膜置于通风橱中,放置两周挥干表面残留溶剂,得到干燥的负载nZnO纳米纤维膜。
(5)按上述方法制备负载有nZnO的PCL纳米纤维膜,其表面形貌如图2所示,可以看出纤维直径分布均匀,相对于纯纺PCL纳米纤维,负载nZnO之后纤维直径变细,通过image J分析可知纳米纤维平均直径减小至179.97±40.01nm
实施案例3:
(1)精确称取1.5gPCL固体颗粒,加入10mL的HFIP溶液,置于磁力搅拌器上,室温条件搅拌12h使PCL充分溶解,配成浓度为15%(w/v)的纺丝液。
(2)在上述纺丝液中加入nZnO粉末,并置于磁力搅拌器上室温搅拌12h,然后将置于超声清洗机中进行超声20min,超声3次,获得含有nZnO的PCL纺丝溶液
(3)在上述溶液中添加1gLBE并置于磁力搅拌器上搅拌,使LBE充分溶解,得到载有10%的LBE和氧化锌的静电纺丝前驱液。
(4)将上述纺丝液转移至10mL带有平口针头的注射器中,通过纺丝装置进行高压静电纺丝,静电纺丝参数设置为:电压20KV、供料速度为0.6mL/h、接收距离为18cm、纺丝环境温度为30℃、纺丝时间为12h,通过滚筒接收器将纳米纤维膜收集到锡箔纸上,得到负载有10%LBE和氧化锌的纳米纤维膜。
(5)将上述所制备的纳米纤维膜置于通风橱中,放置两周,挥干表面残留溶剂,得到干燥的载有10%LBE和氧化锌的纳米纤维膜。
(6)按上述方法制备负载有10%的LBE和氧化锌的纳米纤维膜,其表面形貌如图3所示,可以看出纤维分布相对均匀,具有明显的三维网络结构,纤维之间因为些许黏连出现细丝,通过image J分析可知纳米纤维平均直径为347.7±36.76nm,相对于未负载LBE的纳米纤维直径有所增加。
实施案例4:
(1)精确称取1.5gPCL固体颗粒,加入10mL的HFIP溶液,置于磁力搅拌器上,室温条件搅拌12h使PCL充分溶解,配成浓度为15%(w/v)的纺丝液。
(2)在上述纺丝液中加入nZnO粉末,并置于磁力搅拌器上室温搅拌12h,然后将置于超声清洗机中进行超声20min,超声3次,获得含有nZnO的PCL纺丝溶液
(3)在上述溶液中添加0.25gLBE并置于磁力搅拌器上搅拌,使LBE充分溶解,得到载有2.5%的LBE和氧化锌的静电纺丝前驱液。
(4)将上述纺丝液转移至10mL带有平口针头的注射器中,通过纺丝装置进行高压静电纺丝,静电纺丝参数设置为:电压20KV、供料速度为0.6mL/h、接收距离为18cm、纺丝环境温度为30℃、纺丝时间为12h,通过滚筒接收器将纳米纤维膜收集到锡箔纸上,得到负载有2.5%LBE和氧化锌的纳米纤维膜。
(5)将上述所制备的纳米纤维膜置于通风橱中,放置两周挥干表面残留溶剂,得到干燥的载有2.5%LBE和氧化锌的纳米纤维膜。
实施案例5:
(1)精确称取1.5gPCL固体颗粒,加入10mL的HFIP溶液,置于磁力搅拌器上,室温条件搅拌12h使PCL充分溶解,配成浓度为15%(w/v)的纺丝液。
(2)在上述纺丝液中加入nZnO粉末,并置于磁力搅拌器上室温搅拌12h,然后将置于超声清洗机中进行超声20min,超声3次,获得含有nZnO的PCL纺丝溶液
(3)在上述溶液中添加0.5gLBE并置于磁力搅拌器上搅拌,使LBE充分溶解,得到载有5%的LBE和氧化锌的静电纺丝前驱液。
(4)将上述纺丝液转移至10mL带有平口针头的注射器中,通过纺丝装置进行高压静电纺丝,静电纺丝参数设置为:电压20KV、供料速度为0.6mL/h、接收距离为18cm、纺丝环境温度为30℃、纺丝时间为12h,通过滚筒接收器将纳米纤维膜收集到锡箔纸上,得到负载有5%LBE和氧化锌的纳米纤维膜。
(5)将上述所制备的纳米纤维膜置于通风橱中,放置两周挥干表面残留溶剂,得到干燥的载有5%LBE和氧化锌的纳米纤维膜。
实施案例6:
(1)精确称取1.5gPCL固体颗粒,加入10mL的HFIP溶液,置于磁力搅拌器上,室温条件搅拌12h使PCL充分溶解,配成浓度为15%(w/v)的纺丝液。
(2)在上述纺丝液中加入nZnO粉末,并置于磁力搅拌器上室温搅拌12h,然后将置于超声清洗机中进行超声20min,超声3次,获得含有nZnO的PCL纺丝溶液
(3)在上述溶液中添加0.75g LBE并置于磁力搅拌器上搅拌,使LBE充分溶解,得到载有7.5%的LBE和氧化锌的静电纺丝前驱液。
(4)将上述纺丝液转移至10mL带有平口针头的注射器中,通过纺丝装置进行高压静电纺丝,静电纺丝参数设置为:电压20KV、供料速度为0.6mL/h、接收距离为18cm、纺丝环境温度为30℃、纺丝时间为12h,通过滚筒接收器将纳米纤维膜收集到锡箔纸上,得到负载有7.5%LBE和氧化锌的纳米纤维膜。
(5)将上述所制备的纳米纤维膜置于通风橱中,放置两周,挥干表面残留溶剂,得到干燥的载有7.5%LBE和氧化锌的纳米纤维膜。
(6)分别将实施案例1、案例2、案例3、案例4、案例5、案例6中干燥后纳米纤维膜剪成2cm×3cm的条形,平铺在样品台上,使用移液枪在膜表面滴加3μL蒸馏水,如图4所示,纯纺PCL纳米纤维膜的接触角稳定在136.9±1.3°,加入nZnO后,接触角减小至122±5°,当负载LBE后纳米纤维膜的接触角在3s、6s、9s和12s处的接触角均小于90°,表现出良好的润湿性能,作为医用敷料能为伤口提供湿润的愈合环境,促进愈合。
实施案例7:
分别将实施案例1、案例2、案例3、案例4、案例5、案例6中干燥后纳米纤维膜剪成大小适中的圆片,并固定在瓶口直径40mm、含水量为30mL的瓶口上,置于在37℃、相对湿度为35%的环境中放置24h后将瓶子取出。经计算可知负载nZnO和LBE前后的纳米纤维膜的水蒸气透过率在3500-4000g/m2/d之间(图5,A:PCL、B:PCL/ZnO、C-D:含LBE和ZnO的纳米纤维膜),说明负载nZnO和LBE的纳米纤维膜在提供湿润愈合环境的同时,还能进行气体交换,有利于细胞呼吸。
实施案例8:
分别将实施案例1、案例2、案例3、案例4、案例5、案例6中干燥后的纳米纤维膜切割成条带状(30×5mm)。利用测厚仪测出纳米纤维膜的厚度,并以10mm/min的拉伸速度进行拉伸实验。通过纤维膜的断裂强度公式计算可知,PCL纤维膜在加入nZnO后,断裂强度由7.98±0.66MPa增加到8.72±1.12MPa,而断裂伸长率从36.52±7.10%降低到27.54±3.33%。加入少量的(2.5%)LBE后,纤维膜断裂强度降低至5.95±0.20MPa,断裂伸长率提高到64.99±15.59%。随着LBE浓度的增加,纤维膜的断裂强度增大,断裂伸长先增加后减小,当LBE的浓度为10%时,纤维膜的断裂强力达到最大值10.47±1.29MPa,断裂伸长率为48.79±7.37%,纤维膜的力学性均能满足伤口敷料的要求。
实施案例9:
分别精确50mg实施案例3、案例4、案例5、案例6中干燥后纳米纤维膜,浸入5ml乙醇中,并置于100r/min、37℃的恒温摇床中5h。然后取0.5ml浸出液加入2mL DPPH溶液中,在黑暗中保持30min。用紫外可见光分光光度计测量混合溶液在517nm处的吸光度,通过计算DPPH自由基清除率可知,负载不同含量的LBE(2.5%、5%、7.5%、10%)的纳米纤维膜对自由基清除率分别为30.46%、37.05%、56.51%、76.78%,表现出良好的抗自由基活性。
实施案例10:
分别将实施案例1、案例2、案例3、案例4、案例5、案例6中干燥后纳米纤维膜剪成1×1cm的正方形,正反面紫外灭菌处理后,平铺在已接种菌液之后的固体培养基表面,37℃培养16-24h,观察抑菌情况。如图6所示,相对PCL纳米纤维膜,负载有nZnO和LBE的纳米纤维膜对S.aureus和E.coli表现出了不同程度的抑制效果,在伤口敷料方面,表现出很大的应用潜力。
实施案例11:
分别精确称取实施案例1、案例2、案例3、案例4、案例5、案例6中干燥后纳米纤维膜(20mg),紫外杀菌处理后,并将其浸泡在2mL细胞培养液中24h。将小鼠成纤维细胞(L929)的细胞悬浮液(100μL)接种到96孔板中,并在37℃、5%CO2的环境中培养至孔底覆盖单层细胞,然后加入纳米纤维膜浸出液继续培养24和48h,加入CCK8溶液继续培养4h,用酶标仪测量每个孔的光密度值,如图7所示,纯纺PCL和负载LBE和nZnO之后的纳米纤维膜的吸光度均大于对照组,LBE和ZnO的协同作用促进了L929细胞增殖,证明了,含LBE和氧化锌的纳米纤维膜应用于伤口敷料具有良好的生物安全性。
Claims (7)
1.一种含LBE和氧化锌纳米纤维膜的制备方法,其特征是:A)将聚己内酯溶解在六氟异丙醇溶剂中,得到聚己内酯溶液;B)称取粒径≤20nm的nZnO加入步骤A制备所得的溶液中均匀分散;C)向步骤B所制备的分散液中添加LBE,磁力搅拌溶解得到纺丝前驱液;D)将步骤C制备的纺丝前驱液进行静电纺丝,得到含有LBE和氧化锌的纳米纤维膜;所述纺丝前驱液中nZnO的质量百分浓度为2wt%,LBE的浓度为7.5~10%(w/v),且随着所述纺丝前驱液中LBE的浓度增加,所述纳米纤维膜的断裂强度增加;所述LBE按下列方法制备:在75°C的水浴条件下利用浓度为80%的乙醇对枸杞粉末进行回流提取3次,每次2h,抽滤合并滤液,滤液经过真空旋转蒸发至20~35mL,用等量的石油醚萃取三次,静置,取下层溶液继续旋转蒸发至干,即得到LBE。
2.根据权利要求1所述的含LBE和氧化锌纳米纤维膜的制备方法,其特征在于,所述聚己内酯的分子量为80000。
3.根据权利要求1所述的含LBE和氧化锌纳米纤维膜的制备方法,其特征在于,所述聚己内酯浓度为12~15%(w/v)。
4.根据权利要求1所述的含LBE和氧化锌纳米纤维膜的制备方法,其特征在于,步骤A、步骤B、步骤C的搅拌温度为室温、磁力搅拌速度为500r/min、搅拌12~24h。
5.根据权利要求1所述的含LBE和氧化锌纳米纤维膜的制备方法,其特征在于,所述步骤B的分散方法采用超声分散20min,超声功率为50W。
6.根据权利要求1所述的含LBE和氧化锌纳米纤维膜的制备方法,其特征在于,所述的静电纺丝工艺是将前驱液装入带有平口针头的10mL规格注射器中,在电压为18~22kV、针尖到滚筒的距离为15~20cm、纺丝速度为0.5~1mL/h、针头内径0.7~0.9mm、温度为25~30℃、相对湿度小于30%的条件下,进行静电纺丝,纺丝8~16h,置于通风橱中挥干表面残留溶剂,得到含LBE和氧化锌纳米纤维膜。
7.根据权利要求1所述的含LBE和氧化锌纳米纤维膜的制备方法制得的纳米纤维膜作为伤口敷料的应用。
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