CN111321514A - 聚乙烯醇-纳米银敷料及制备方法和用途 - Google Patents
聚乙烯醇-纳米银敷料及制备方法和用途 Download PDFInfo
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- CN111321514A CN111321514A CN202010213735.8A CN202010213735A CN111321514A CN 111321514 A CN111321514 A CN 111321514A CN 202010213735 A CN202010213735 A CN 202010213735A CN 111321514 A CN111321514 A CN 111321514A
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- Prior art keywords
- polyvinyl alcohol
- dressing
- nano silver
- acid
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
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- 238000002360 preparation method Methods 0.000 title abstract description 10
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Abstract
本发明涉及一种聚乙烯醇–纳米银敷料及制备方法和用途，所述敷料由聚乙烯醇、纳米银和生物相容性多元酸组成。该敷料不含抗生素药物，无有机溶剂和有毒化学物质残留，具有抗菌、促愈、生物相容性好等优点，可作为伤口创面、溃疡创面、各种细菌感染以及难愈性创面的创面敷料。
Description
技术领域
本发明涉及一种生物医用材料，特别涉及一种聚乙烯醇–纳米银敷料及制备方法和用途。
背景技术
敷料可以改善创面微环境，对创面愈合起着至关重要的作用，理想的创面敷料应具有无毒、生物相容性好、加速创面愈合、防止创面感染等特性。目前临床上普遍采用的是含抗生素药物的敷料，但抗生素的长期使用会使细菌产生耐药性。已上市的创面敷料难以满足临床需求。
聚乙烯醇是一种水溶性高分子，其分子结构中含有大量的羟基，具有亲水性好、生物相容性好、无毒、可生物降解等特点，在皮肤、软骨、角膜等组织的移植替换和修复重建等医学领域中具有广泛的应用。但通过静电纺丝法直接制备的聚乙烯醇纳米纤维膜易溶于水，不适合作为创面敷料，需要经过进一步交联来解决其溶于水、机械性能差、难于直接应用的缺点。
银及其化合物在杀菌、消毒和抗炎等方面具有广泛的应用，而且细菌对银不存在耐药性。另外，银还可以促进伤口的愈合。通过简单的沉积、浸泡或直接负载等方法所得的含银（银化合物或银纳米粒子）敷料中银的释放难以控制，不仅影响了敷料的抗菌性能，而且会产生大量银进入体内循环的可能，增加了使用风险。
通常采用的戊二醛等化学交联剂具有毒性、极易残留，限制了交联后纤维膜的应用范围。而采用的直接将纳米银粉加入纺丝溶液中所制备的纳米银静电纺丝敷料中的纳米银容易脱落，造成局部银含量过高从而产生毒副作用。
发明内容
本发明的目的是提供一种聚乙烯醇–纳米银敷料及制备方法和用途，该敷料不含抗生素药物、有机溶剂以及有毒化学物质残留，并且敷料中纳米银均匀固定于纺丝的三维结构中不易大量脱落，避免局部银浓度过高而产生的毒副作用，具有抗菌、促愈、生物相容性好等优点，可作为伤口创面、溃疡创面、各种细菌感染以及难愈性创面的创面敷料。
本发明的技术方案是：
聚乙烯醇–纳米银敷料，其特征在于：该敷料由聚乙烯醇、纳米银和生物相容性多元酸组成，所述敷料通过聚乙烯醇与生物相容性多元酸形成交联纳米纤维。
所述聚乙烯醇为分子量为10000～1000000的聚乙烯醇。
所述多元酸为含有羧基的小分子二元酸或含有羧基的高分子。
所述含有羧基的小分子二元酸为柠檬酸或马来酸或富马酸或丁二酸。
所述含有羧基的高分子为聚丙烯酸或透明质酸或聚苯乙烯磺酸-马来酸共聚物。
上述聚乙烯醇–纳米银敷料的制备方法，其特征在于，有以下步骤：
1）纳米银溶液的制备：
将硝酸银和生物相容性多元酸溶于去离子水中，其硝酸银：生物相容性多元酸的质量比为1:0.1～50，将该混合溶液加热至30～100℃，得到稳定的纳米银溶液；
2）静电纺丝水溶液的配制：
步骤1）得到的纳米银溶液中加入聚乙烯醇，充分搅拌溶解，得到纺丝溶液；
3）静电纺丝纳米纤维的制备：
将步骤2）中得到的纺丝溶液加入静电纺丝机的供液单元，设置纺丝电压10～35 kV，接收距离10～30 cm，在静电纺丝机的接收装置上得到聚乙烯醇–纳米银静电纺丝膜；
4）静电纺丝纳米纤维的热交联：
将步骤3）中得到的聚乙烯醇–纳米银静电纺丝膜在烘箱中加热，交联。
步骤3）所述纺丝供液单元中有纺丝液，该纺丝液为步骤1）所述的多元酸。
纺丝液：聚乙烯醇的质量比为1:5～1: 100。
步骤4）所述加热交联温度为100～150摄氏度；加热交联时间为0.5～12小时。
上述的聚乙烯醇–纳米银敷料用于治疗伤口创面、溃疡创面、细菌感染、难愈性创面的敷料的用途。
本发明所述的静电纺丝膜中纳米纤维的随机排列产生多孔间隙，使其具有与天然细胞外基质类似的结构，不仅为细胞生长提供一个良好的支架，还可以促进创面液体吸收。静电纺丝技术可以低成本、快速方便的制备各种聚合物纳米纤维。通过向纺丝溶液中加入一种或多种药物，可以获得多功能纳米纤维膜，为抗菌促愈纳米纤维膜敷料的制备提供了可能。
本发明所述敷料利用静电纺丝技术将含有以上成分的水溶液加工制作成纳米纤维膜，通过高温交联后制得交联纳米纤维膜敷料，所得到的含纳米银抗菌促愈敷料具有孔隙率高、透气性好等特点。该敷料制备过程中以水为溶剂，采用的原料生物相容性好，无有机溶剂和有毒化学物质残留。
本发明中纳米银的稳定剂多元酸同时作为静电纺丝纳米纤维膜的交联剂，经高温热交联后可将纳米银限定于纳米纤维中防止纳米银的聚集、脱落，提高抗菌性能的同时减少大量银进入体内带来的毒副作用。
本发明的有益效果：
本发明利用静电纺丝技术将聚乙烯醇与纳米银结合制备功能性纳米纤维膜，所得纤维膜具有抗菌、促愈、生物相容性好等优点。
本发明采用生物相容性原料进行纺丝和进一步热交联，工艺简单，所得纳米纤维膜不仅可防止水溶解，也具有较好的生物相容性。
本发明中多元酸既作为纳米银的稳定剂也同时作为交联剂，纳米银被限制于交联形成的三维高分子链网络中解决了纳米银的脱落、聚集问题，接触创面后缓慢释放银离子抗菌促愈的同时可防止脱落的纳米银进入体内产生毒副作用。
本发明所述敷料成本低廉、制备工艺简单，应用广泛，可作为伤口创面、溃疡创面、各种细菌感染以及难愈性创面的创面敷料。
附图说明
图1是本发明实施例1所述聚乙烯醇–纳米银敷料的扫描电子显微镜图；
图2是本发明实施例1所述聚乙烯醇聚乙烯醇–纳米银敷料纳米银敷料的透射电子显微镜图；
图3为实施例1-5所得为聚乙烯醇聚乙烯醇–纳米银敷料纳米银敷料对大肠杆菌(a)和金黄色葡萄球菌(b)的抗菌效果图，其中1–5号分别是实施例1–5的聚乙烯醇-纳米银敷料的抗菌效果，6号为不含银的聚乙烯醇聚苯乙烯磺酸–马来酸共聚物敷料的对照组；
图4 为C57小鼠不同时相点的创面残留情况。
具体实施方式
本实施例所有化学试剂均购于sigma公司。
实施例1
马来酸纳米银溶液的制备：
1）取0.1 g硝酸银溶解于90mL去离子水中，将该溶液加热至100℃，快速加入10 mL 8%（0.8g）的马来酸溶液进行还原，反应1小时后得到均一透明、稳定的马来酸纳米银溶液；
2）静电纺丝溶液的配制：
步骤1）得到的马来酸纳米银溶液中加入聚乙烯醇，充分搅拌溶解，得到均一的纺丝溶液；
3）静电纺丝纳米纤维的制备：
步骤2）中得到的纺丝溶液加入静电纺丝机的供液单元，设置纺丝电压15 kV，接收距离25 cm，在接收装置上得到聚乙烯醇-纳米银静电纺丝膜；
4）静电纺丝纳米纤维的交联：
步骤3）得到的聚乙烯醇-纳米银静电纺丝膜在烘箱中130摄氏度加热交联2小时。得到本发明所述聚乙烯醇-纳米银敷料（参见图1-图2。
实施例2
1）透明质酸纳米银溶液的制备：
0.1 g硝酸银和0.5 g透明质酸（分子量3 kDa）溶于100 mL水中，加热至80℃对溶液进行还原，反应8小时后得到均一透明的透明质酸纳米银溶液；
2）静电纺丝溶液的配制：
步骤1）到的透明质酸稳定的纳米银溶液10 mL中加入1 g聚乙烯醇，充分搅拌溶解，得到均一纺丝溶液；
3）静电纺丝纳米纤维的制备：
步骤2）得到的纺丝溶液加入静电纺丝机的供液单元，设置纺丝电压30 kV，接收距离25cm，在接收装置上得到聚乙烯醇-纳米银静电纺丝膜；
4）静电纺丝纳米纤维的交联：
步骤3）得到的聚乙烯醇-纳米银静电纺丝膜在烘箱中120摄氏度加热交联3小时。得到本发明所述聚乙烯醇-纳米银敷料。
实施例3
1）聚丙烯酸稳定剂的纳米银溶液的制备：
0.1 g硝酸银溶解于90 mL去离子水中，将该溶液加热至100℃，快速加入10 mL 6%（0.6g）的聚丙烯酸（分子量1800）溶液进行还原，反应1小时后得到均一透明的聚丙烯酸稳定的纳米银溶液；
2）静电纺丝溶液的配制：
步骤1）得到的聚丙烯酸稳定的纳米银溶液中10 mL加入1 g聚乙烯醇，充分搅拌溶解，得到均一纺丝溶液；
3）静电纺丝纳米纤维的制备：
步骤2）得到的纺丝溶液加入静电纺丝机的供液单元，设置纺丝电压20 kV，接收距离15cm，在接收装置上得到聚乙烯醇-纳米银静电纺丝膜；
4）静电纺丝纳米纤维的交联：
步骤3）中得到的聚乙烯醇-纳米银静电纺丝膜在烘箱中150摄氏度加热交联1小时。得到本发明所述聚乙烯醇-纳米银敷料。
实施例4
1）柠檬酸纳米银溶液的制备：
0.1 g硝酸银溶解于90 mL去离子水中，将该溶液加热至100℃，快速加入10 mL 5%的柠檬酸-柠檬酸钠（0.25g柠檬酸以及0.25g柠檬酸钠）混合溶液进行还原（其中柠檬酸和柠檬酸钠质量比为1:1），反应1小时后得到均一透明的柠檬酸稳定的纳米银溶液；
2）静电纺丝溶液的配制：
步骤1）得到的柠檬酸稳定的纳米银溶液10 mL中加入1 g聚乙烯醇，充分搅拌溶解，得到均一纺丝溶液；
3）静电纺丝纳米纤维的制备：
步骤2）得到的纺丝溶液加入静电纺丝机(NANO SPIDER捷克Elmarco公司)的供液单元，设置纺丝电压30 kV，接收距离25 cm，在接收装置上得到聚乙烯醇-纳米银静电纺丝膜；
4）静电纺丝纳米纤维的交联：
步骤3）得到的聚乙烯醇-纳米银静电纺丝膜在烘箱中120摄氏度加热交联3小时。得到本发明所述聚乙烯醇-纳米银敷料。
实施例5
1）聚苯乙烯磺酸-马来酸共聚物稳定的纳米银溶液的制备：
0.5 g硝酸银和2.0 g聚苯乙烯磺酸-马来酸共聚物（聚苯乙烯磺酸-马来酸比例为1:1，聚苯乙烯磺酸分子量20000）溶于100 mL去离子水中，通过将该混合溶液加热至70℃对硝酸银进行还原，反应12小时后得到均一透明的聚苯乙烯磺酸-马来酸共聚物稳定的纳米银溶液；
2）静电纺丝溶液的配制：
步骤1）得到的聚苯乙烯磺酸-马来酸共聚物稳定的纳米银溶液10 mL中加入1 g聚乙烯醇，充分搅拌溶解，得到均一纺丝溶液；
3）静电纺丝纳米纤维的制备：
步骤2）得到的纺丝溶液加入静电纺丝机的供液单元，设置纺丝电压20 kV，接收距离30cm，在接收装置上得到聚乙烯醇-纳米银静电纺丝膜；
4）静电纺丝纳米纤维的交联：
步骤3）得到的聚乙烯醇-纳米银静电纺丝膜在烘箱中100摄氏度加热交联6小时。
得到本发明所述聚乙烯醇-纳米银敷料。
实施例6
聚乙烯醇-纳米银敷料的抗菌实验
将实施例1-5所述的聚乙烯醇-纳米银敷料，分别剪成1cm的纤维膜片，再分别贴于大肠杆菌ATCC25922和金黄色葡萄球菌ATCC25923的平板上，37摄氏度培养24h后观察抑菌圈。实验结果表明聚乙烯醇-纳米银敷料具有抗菌能力，如图3所示。
实施例7
聚乙烯醇-纳米银敷料的创面促愈实验
选用C57小鼠用1%戊巴比妥钠腹腔麻醉后，利用皮肤活检器制作全层皮肤缺损动物模型，随机分组，每组6只，之后按照分组进行给予敷料。动物单独分笼饲养。选不同的时间点拍照。图4表明各组创面呈渐进性愈合,愈合残留面积逐渐缩小。敷料组于伤后12-13天愈合，对照组提前3-4天愈合，治疗效果优于磺胺嘧啶银。
Claims (10)
1.一种聚乙烯醇–纳米银敷料，其特征在于：该敷料由聚乙烯醇、纳米银和生物相容性多元酸组成，所述敷料通过聚乙烯醇与生物相容性多元酸形成交联纳米纤维。
2.根据权利要求1所述的敷料，其特征在于：所述聚乙烯醇为分子量为10000～1000000的聚乙烯醇。
3.根据权利要求1所述的敷料，其特征在于：所述多元酸为含有羧基的小分子二元酸或含有羧基的高分子。
4.根据权利要求3所述的敷料，其特征在于：所述含有羧基的小分子二元酸为柠檬酸或马来酸或富马酸或丁二酸。
5.根据权利要求4所述的敷料，其特征在于：所述含有羧基的高分子为聚丙烯酸或透明质酸或聚苯乙烯磺酸-马来酸共聚物。
6.权利要求1–5任一所述聚乙烯醇–纳米银敷料的制备方法，其特征在于，有以下步骤：
1）纳米银溶液的制备：
将硝酸银和生物相容性多元酸溶于去离子水中，其硝酸银：生物相容性多元酸的质量比为1:0.1～50，将该混合溶液加热至30～100℃，得到稳定的纳米银溶液；
2）静电纺丝水溶液的配制：
步骤1）得到的纳米银溶液中加入聚乙烯醇，充分搅拌溶解，得到纺丝溶液；
3）静电纺丝纳米纤维的制备：
将步骤2）中得到的纺丝溶液加入静电纺丝机的供液单元，设置纺丝电压10～35 kV，接收距离10～30 cm，在静电纺丝机的接收装置上得到聚乙烯醇–纳米银静电纺丝膜；
4）静电纺丝纳米纤维的热交联：
将步骤3）中得到的聚乙烯醇–纳米银静电纺丝膜在烘箱中加热，交联。
7.根据权利要求6所述的方法，其特征在于：步骤3）所述纺丝供液单元中有纺丝液，该纺丝液为步骤1）所述的多元酸。
8.根据权利要求7所述的方法，其特征在于：纺丝液：聚乙烯醇的质量比为1:5～1:100。
9.根据权利要求6所述的方法，其特征在于：步骤4）所述加热交联温度为100～150摄氏度；加热交联时间为0.5～12小时。
10.权利要求1–5任一所述的聚乙烯醇–纳米银敷料用于治疗伤口创面、溃疡创面、细菌感染、难愈性创面的敷料的用途。
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