CN111118734A - 一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料及其制备方法与应用 - Google Patents
一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料及其制备方法与应用 Download PDFInfo
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Abstract
本发明属于医药技术领域,具体公开了一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料及其制备方法与应用。所述制备方法,具体包括以下步骤:将聚乙烯醇(PVA)、羧甲基壳聚糖(CMCS)、美洲大蠊浓缩液和水混合均匀,制得含有美洲大蠊活性物质的纺丝液;然后通过静电纺丝制得美洲大蠊缓释医用敷料。相较于传统的医用纱布加敷料或使用涂布的方法制备医用敷料,缓释纳米纤维医用敷料既具有很好的透气性与很高的孔隙率,既可以使伤口保持湿润利于细胞的呼吸作用。纳米纤维可有效阻止空气中的细菌与微粒接触伤口。相较于一般的涂布制备的医用敷料,纳米纤维医用敷料具有良好的透气性和较好的吸收皮肤渗出液。
Description
技术领域
本发明属于医药技术领域,具体涉及一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料及其制备方法与应用。
背景技术
美洲大蠊属昆虫纲蜚蠊亚目蜚蠊科大蠊属,俗称蟑螂,是世界上生命力最强、最古老,至今繁衍最成功的昆虫类群之一。美洲大蠊是传统中药材入药始载于《神农本草经》,现代研究表明其具有抗癌、抗菌、抗炎、促进组织修复等药理作用。美洲大蠊中的化学成分主要有信息素、聚集信息素、氨基酸、昆神经肽、糖类、蛋白质、油脂、核酸类、异黄酮等。
羧甲基壳聚糖及其多种衍生物均具有不同程度的抗感染作用,以壳聚糖六聚糖为最强。小分子的脱乙酰壳聚糖具有质子化铵,质子化铵与细菌带负电荷的细胞膜作用,吸附和聚沉细菌,同时穿透细胞壁进入细胞内,扰乱细菌的新陈代谢及合成而具有抗菌作用。
目前我国大多数医疗机构仍然将传统的棉质纱布作为常用的医用敷料,但传统的医用纱布需要频繁更换,伤口易干燥,目前只有物理隔离功能,且易于渗出物结痂,造成伤口与敷料之间的黏连,引起新组织的二次创伤,也会出现细菌滋生、止血效果差等临床现象。静电纺丝制备的纤维直径小,所形成的纳米纤维膜比表面积大、孔隙率高、纤维呈各向异性。相对其他形式的纤维材料,静电纺丝纳米纤维膜能够满足理想医用敷料的要求,可为增殖细胞提供必要的支撑和引导、高吸液率及半渗透性、优异的止血效果及贴合性,静电纺丝纳米纤维比表面积高使其成为优异的药物载体。
发明内容
为了克服上述现有技术的缺点与不足,本发明的首要目的在于提供一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法。
本发明另一目的在于提供上述方法制备得到的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法。
本发明再一目的在于提供聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法在制备伤口敷料中的应用。
本发明的目的通过下述方案实现:
一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,具体包括以下步骤:将聚乙烯醇(PVA)、羧甲基壳聚糖(CMCS)、美洲大蠊浓缩液和水混合均匀,制得含有美洲大蠊活性物质的纺丝液;然后通过静电纺丝制得美洲大蠊缓释医用敷料。
所述PVA与CMCS的质量比为2~5:1,优选为4:1;所述含有美洲大蠊活性物质的纺丝液中PVA和CMCS的总质量分数为8~15%,优选为10~12%。
所述美洲大蠊浓缩液的固含量为10~50%,优选为30%;所述美洲大蠊浓缩液与水的质量比为1:40~100。
所述混合的温度为50~70℃,混合时间为3~8h;优选地,所述混合的温度为60℃,混合时间为5h。
所述静电纺丝的条件为温度为20~30℃,湿度38~48%RH的下进行实验。设置纺丝条件为:注射速度3~6mm/h,接收距离16~24cm,纺丝电压18~24kV。优选为采用环境温度为28℃,湿度40%RH的下进行实验。设置纺丝条件为:注射速度4.0mm/h,接收距离20cm,纺丝电压23kV。
优选地,静电纺丝完成后,将所得美洲大蠊缓释医用敷料在70~100℃下热处理30~120min,促进交联反应。更优选地,所述热处理的温度为90℃,时间为60min。
一种含美洲大蠊的纳米纤维医用敷料,通过上述方法制备得到。
上述含美洲大蠊的纳米纤维医用敷料在制备伤口敷料中的应用。
本发明相对于现有技术,具有如下的优点及有益效果:
(1)不同于传统的使用医用纱布加敷料或使用涂布的方法制备医用敷料的思路,将美洲大蠊活性成分直接与PVA与CMCS混合制成纺丝液,使用静电纺丝直接制备出具有缓释效果的纳米纤维敷料,使用时直接将纳米纤维敷料覆盖在伤口上。
(2)相较于传统的医用纱布加敷料或使用涂布的方法制备医用敷料,缓释纳米纤维医用敷料既具有很好的透气性与很高的孔隙率,既可以使伤口保持湿润利于细胞的呼吸作用。纳米纤维可有效阻止空气中的细菌与微粒接触伤口。相较于传统织物制成的敷料以及薄膜材料制成的医用敷料,纳米纤维医用敷料具有很强的优势,具有相较于传统织物制成的医用敷料更好的贴敷性,隔绝空气中的灰尘、病原体等。相较于一般的涂布制备的医用敷料,纳米纤维医用敷料具有良好的透气性和较好的吸收皮肤渗出液。
(3)PVA纳米纤维在组织液中十分容易溶解,在组织液中释放出活性物质,使得美洲大蠊活性物质一次性大量在伤口中释放,而将PVA纳米纤维进行热处理之后,纤维中PVA大分子链上的羟基会与CMCS上的羧基发生酯化反应,生成酯基,使得纤维的水溶性下降。由于PVA大分子链上的羟基反应不完全,所以PVA纳米纤维部分溶于水,释放出美洲大蠊活性物质,同时,CMCS也具有很好的抗菌效果,与美洲大蠊活性物质共同发挥作用,而交联好的大分子链疏水,会充当骨架,支撑医用敷料,并且吸附组织液避免渗出物在患处大量聚积,还能有效组织外界病菌入侵。
(4)由于CMCS可纺性较差,与PVA混纺后制备出的纳米纤维,在高温烘燥过程中发生酯化反应,酯化反应是一个缓慢的可逆反应,所以PVA分子链上的羟基反应不完全,纳米纤维医用敷料在伤口组织液中只会部分溶解,逐步释放活性物质,同时CMCS未交联的分子链溶于组织液中起到抗菌效果。
附图说明
图1为实施例1所得纳米纤维医用敷料电镜图。
图2为实施例1中苯丙氨酸在水中的浓度随浸泡时间的变化趋势图。
图3为实施例2中苯丙氨酸在水中的浓度随浸泡时间的变化趋势图。
图4为实施例3中苯丙氨酸在水中的浓度随浸泡时间的变化趋势图。
图5为实施例4中苯丙氨酸在水中的浓度随浸泡时间的变化趋势图。
图6为实施例5中苯丙氨酸在水中的浓度随浸泡时间的变化趋势图。
图7为实施例1~5中所得纳米纤维医用敷料浸润前后强力图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。PVA购买于上海麦克林生化科技有限公司,PVA1788;CMCS购买于国药集团化学试剂有限公司;美洲大蠊浓缩液购买于四川好医生攀西药业有限责任公司。
实施例中所用试剂如无特殊说明均可从市场常规购得。
实施例1
采用环境温度为30℃,湿度40%RH的下进行实验。用电子天平称取10g的PVA,将其装入干净的锥形瓶中,然后将美洲大蠊浓缩液1.5g(已知固含量为30%)加入锥形瓶中,向容量瓶中加入2g CMCS,计算好溶质与溶剂的质量比之后将100g的纯水加入锥形瓶中,在温度为60℃水浴锅中进行搅拌5h后,制备出美洲大蠊@PVA/CMCS纺丝液。设置纺丝条件为:注射速度4.0mm/h,接收距离20cm,纺丝电压为23kV,使用静电纺丝机制备出美洲大蠊@PVA/CMCS纳米纤维膜医用敷料。设置烘燥温度85℃,在烘箱中烘燥30min,经过一定的热处理,促进交联反应,使PVA/CMCS纳米纤维膜耐水性提高。
静电纺丝制备的缓释纳米纤维医用敷料电镜图如图1所示。由于美洲大蠊浓缩液为混合物,我们选取其中苯丙氨酸作为标定物,将0.01克的纳米纤维膜放入到样品管,再注入1mL纯水,控制纳米纤维膜的浸泡时间,使用高效液相色谱仪测试其水溶液中苯丙氨酸的浓度。苯丙氨酸在水中的浓度随浸泡时间的变化趋势如图2所示。缓释纳米纤维医用敷料浸润前后强力如图7所示。
实施例2
采用环境温度为25℃,湿度42%RH的下进行实验。用电子天平称取5g的PVA,将其装入干净的锥形瓶中,然后将美洲大蠊浓缩液0.8g(已知固含量为30%)加入锥形瓶中,向容量瓶中加入2g CMCS,计算好溶质与溶剂的质量比之后将45g的纯水加入锥形瓶中,在温度为60℃水浴锅中进行搅拌5h后,制备出的美洲大蠊@PVA/CMCS纺丝液。设置纺丝条件为:注射速度3.0mm/h,接收距离18cm,纺丝电压为20kV,使用静电纺丝机制备出美洲大蠊@PVA/CMCS纳米纤维膜医用敷料。设置烘燥温度90℃,在烘箱中烘燥60min,经过一定的热处理,促进交联反应,使PVA/CMCS纳米纤维膜耐水性提高。
由于美洲大蠊浓缩液为混合物,我们选取其中苯丙氨酸作为标定物,将0.01克的纳米纤维膜放入到样品管,再注入1mL纯水,控制纳米纤维膜的浸泡时间,使用高效液相色谱仪测试其水溶液中苯丙氨酸的浓度。苯丙氨酸在水中的浓度随浸泡时间的变化趋势如图3所示。缓释纳米纤维医用敷料浸润前后强力如图7所示。
实施例3
采用环境温度为25℃,湿度39%RH的下进行实验。用电子天平称取5g的PVA,将其装入干净的锥形瓶中,然后将美洲大蠊浓缩液0.7g(已知固含量为30%)加入锥形瓶中,向容量瓶中加入1.5g CMCS。计算好溶质与溶剂的质量比之后将40g的纯水加入锥形瓶中,在温度为60℃水浴锅中进行搅拌5h后,制备出美洲大蠊@PVA/CMCS纺丝液。设置纺丝条件为:注射速度5.0mm/h,接收距离20cm,纺丝电压为21kV,使用静电纺丝机制备出美洲大蠊@PVA/CMCS纳米纤维膜医用敷料。设置烘燥温度80℃,在烘箱中烘燥90min,经过一定的热处理,促进交联反应,使PVA/CMCS纳米纤维膜耐水性提高。
由于美洲大蠊浓缩液为混合物,我们选取其中苯丙氨酸作为标定物,将0.01克的纳米纤维膜放入到样品管,再注入1mL纯水,控制纳米纤维膜的浸泡时间,使用高效液相色谱仪测试其水溶液中苯丙氨酸的浓度。苯丙氨酸在水中的浓度随浸泡时间的变化趋势如图4所示。缓释纳米纤维医用敷料浸润前后强力如图7所示。
实施例4
采用环境温度为30℃,湿度45%RH的下进行实验。用电子天平称取5g的PVA,将其装入干净的锥形瓶中,然后将美洲大蠊浓缩液0.5(已知固含量为30%)加入锥形瓶中,向容量瓶中加入1g CMCS。,计算好溶质与溶剂的质量比之后将50g的纯水加入锥形瓶中,在温度为60℃水浴锅中进行搅拌6h后,制备出美洲大蠊@PVA/CMCS纺丝液。设置纺丝条件为:注射速度6.0mm/h,接收距离22cm,纺丝电压为23kV,使用静电纺丝机制备出美洲大蠊@PVA/CMCS纳米纤维膜医用敷料。设置烘燥温度90℃,在烘箱中烘燥120min,经过一定的热处理,促进交联反应,使PVA/CMCS纳米纤维膜耐水性提高。
由于美洲大蠊浓缩液为混合物,我们选取其中苯丙氨酸作为标定物,将0.01克的纳米纤维膜放入到样品管,再注入1mL纯水,控制纳米纤维膜的浸泡时间,使用高效液相色谱仪测试其水溶液中苯丙氨酸的浓度。苯丙氨酸在水中的浓度随浸泡时间的变化趋势如图5所示。缓释纳米纤维医用敷料浸润前后强力如图7所示。
实施例5
采用环境温度为28℃,湿度40%RH的下进行实验。用电子天平称取5g的PVA,将其装入干净的锥形瓶中,然后将美洲大蠊浓缩液1.5g(已知固含量为30%)加入锥形瓶中,向容量瓶中加入0.5gCMCS。,计算好溶质与溶剂的质量比之后将55g纯水加入锥形瓶中,在温度为60℃水浴锅中进行搅拌5h后,制备出美洲大蠊@PVA/CMCS纺丝液。设置纺丝条件为:注射速度6.0mm/h,接收距离20cm,纺丝电压为23kV,使用静电纺丝机制备出美洲大蠊@PVA/CMCS纳米纤维膜医用敷料。设置烘燥温度70℃,在烘箱中烘燥30min,经过一定的热处理,促进交联反应,使PVA/CMCS纳米纤维膜耐水性提高。
由于美洲大蠊浓缩液为混合物,我们选取其中苯丙氨酸作为标定物,将0.01克的纳米纤维膜放入到样品管,再注入1mL纯水,控制纳米纤维膜的浸泡时间,使用高效液相色谱仪测试其水溶液中苯丙氨酸的浓度。苯丙氨酸在水中的浓度随浸泡时间的变化趋势如图6所示。缓释纳米纤维医用敷料浸润前后强力如图7所示。
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、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 (9)
1.一种聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于具体包括以下步骤:
将聚乙烯醇、羧甲基壳聚糖、美洲大蠊浓缩液和水混合均匀,制得含有美洲大蠊活性物质的纺丝液;然后通过静电纺丝制得美洲大蠊缓释医用敷料。
2.根据权利要求1所述的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于:
所述PVA与CMCS的质量比为2~5:1;所述含有美洲大蠊活性物质的纺丝液中PVA和CMCS的总质量分数为8~15%。
3.根据权利要求1所述的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于:
所述美洲大蠊浓缩液的固含量为10~50%;所述美洲大蠊浓缩液与水的质量比为1:40~100。
4.根据权利要求1所述的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于:
所述PVA与CMCS的质量比为4:1;所述含有美洲大蠊活性物质的纺丝液中PVA和CMCS的总质量分数为10~12%;所述美洲大蠊浓缩液的固含量为30%。
5.根据权利要求1所述的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于:所述混合的温度为50~70℃,混合时间为3~8h。
6.根据权利要求1所述的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于:静电纺丝完成后,将所得美洲大蠊缓释医用敷料在70~100℃下热处理30~120min。
7.根据权利要求1所述的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料的制备方法,其特征在于:设置纺丝条件为:注射速度3~6mm/h,接收距离16~24cm,纺丝电压18~24kV。
8.根据权利要求1~7任一项所述方法制备得到的聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料。
9.根据权利要求8所述聚乙烯醇/羧甲基壳聚糖纳米纤维医用敷料在制备伤口敷料中的应用。
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