CN115212345A - 一种多酚交联天然多糖基水凝胶敷料及其制备方法和应用 - Google Patents
一种多酚交联天然多糖基水凝胶敷料及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供了一种多酚交联天然多糖基水凝胶敷料及其制备方法和应用，属于生物医用材料领域。本发明的技术方案要点为：首先是具有邻二醇结构的天然多糖被高碘酸钠氧化得到醛基多糖，然后与接枝有抗菌、抗氧化基团的氨基天然多糖衍生物复合，通过形成Schiff碱交联即可得到多功能水凝胶材料。本发明通过对天然多糖的功能化接枝改性，从而赋予水凝胶内在的多功能性，避免了抗菌等药物使用带来的耐药性问题，在长效促进复杂创面愈合方面具有重要的应用价值。
Description
技术领域
本发明属于生物医用材料技术领域，具体涉及一种多酚交联天然多糖基水凝胶敷料及其制备方法和应用。
背景技术
皮肤创伤，主要包括急性创伤和慢性炎症，这些创伤给患者们带来了各种各样的问题。 皮肤的创伤会导致皮肤丧失某些重要功能，特别是损伤保护人体免受外部致病环境的屏障，从而导致出血和感染，并且会延迟伤口愈合过程。在这个过程中，就需要一些紧急的治疗措施，例如止血、消炎、皮肤细胞的快速增殖和重塑，有利于加速伤口愈合，恢复百分之百的正常皮肤功能。迄今为止，人们已经研发出各种各样的伤口敷料。在诸多类型的伤口敷料中，水凝胶敷料具有独特的优势，其可以保持伤口处的湿润，多孔结构不仅有利于营养物质的传输，还可吸收伤口部位的渗出液等。水凝胶作为一种良好的载体，可以负载抗生素及过渡金属化合物纳米材料等，用以实现特定功能以促进伤口愈合；但是该方法会产生耐药性等副作用，而设计制备具有内在多功能性的水凝胶伤口敷料在临床应用方面具有重要的意义。
公开号为CN108976758A的发明创造公开了一种光敏性的聚乙二醇基抗菌水凝胶敷料及其制备方法，该水凝胶敷料以聚乙二醇为基材，通过光敏性共价键将硫酸庆大霉素接枝到凝胶网络中，并可实现药物在创面处的紫外光响应性释放。该聚乙二醇基水凝胶敷料具有良好的抗菌性能，并可以实现高校便捷的光响应操作。然而该方法制得的聚乙二醇基抗菌水凝胶是通过负载抗生素来实现抗菌功能，长期使用会产生耐药性等副作用，在伤口愈合等生物医用材料领域有必要对伤口敷料进行改进。
发明内容
本发明的目的在于针对现有水凝胶敷料存在的不足，提供了一种多酚交联天然多糖基具水凝胶敷料及其制备方法，该水凝胶敷料具有内在的有抗菌、抗氧化、促愈合的多功能性。具体方法是将苯硼酸接枝的天然多糖与天然多酚通过硼酸酯交联得到多功能水凝胶敷料；天然多酚不仅赋予了该水凝胶抗菌、抗氧化性能，其还赋予了水凝胶组织粘附性，能够较好地作为医用水凝胶伤口敷料应用于促进创伤愈合。
本发明为实现上述目的采用如下技术方案，一种多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于具体步骤为：
步骤S1：将含有氨基的天然多糖或含有醛基的天然多糖溶于去离子水中得到氨基多糖溶液或醛基多糖溶液，其中含有氨基的天然多糖为壳聚糖、羧甲基壳聚糖、羧乙基壳聚糖或羟乙基壳聚糖中的一种或多种；
步骤S2：将3-甲酰基苯硼酸或4-甲酰基苯硼酸加入到步骤S1得到的氨基多糖溶液中并于室温搅拌至全部溶解得到溶液A，或者将3-氨基苯硼酸或4-氨基苯硼酸加入到步骤S1得到的醛基多糖溶液中并于室温搅拌至全部溶解得到溶液B；
步骤S3：将天然多酚溶于去离子水中得到多酚溶液，其中天然多酚为原花青素、表没食子儿茶素没食子酸酯、表没食子儿茶素、表儿茶酚没食子酸、单宁酸、鞣花酸、芦丁或棉酚中的一种或多种；
步骤S4：将步骤S2得到的溶液A或溶液B与步骤S3得到的多酚溶液混匀，再于室温静置即可得到具有内在抗菌、抗氧化、促愈合功能性的多酚交联天然多糖基水凝胶敷料。
进一步限定，步骤S1中所述含有醛基的天然多糖的具体制备过程为：
步骤S101：将含有邻二醇结构的天然多糖溶于去离子水中得到含有邻二醇结构的天然多糖溶液，其中含有邻二醇结构的天然多糖为海藻酸钠、透明质酸钠、魔芋胶、瓜尔豆胶、阿拉伯树胶、葡聚糖、纤维素、硫酸软骨素或肝素中的一种或多种；
步骤S102：将高碘酸钠溶于去离子水中得到高碘酸钠溶液；
步骤S103：将步骤S102得到的高碘酸钠溶液加入到步骤S101得到的含有邻二醇结构的天然多糖溶液中混匀，于室温下避光搅拌反应，再向反应液中加入乙二醇继续反应，反应完成后将反应液装入透析袋，放入去离子水中透析后冻干得到含有醛基的天然多糖。
进一步限定，步骤S103中所述高碘酸钠与含有邻二醇结构的天然多糖的摩尔比为0.2~2:1。
进一步限定，步骤S1中所述氨基多糖溶液或醛基多糖溶液的浓度为2~150mg/mL。
进一步限定，步骤S2中所述3-甲酰基苯硼酸或4-甲酰基苯硼酸与氨基多糖溶液中氨基的摩尔比为0.05~0.2:1，3-氨基苯硼酸或4-氨基苯硼酸与醛基多糖溶液中醛基的摩尔比为0.05~0.4:1。
进一步限定，步骤S3中所述多酚溶液的浓度为5~100mg/mL。
进一步限定，步骤S4中所述溶液A或溶液B与多酚溶液的投料配比满足：步骤S2得到的溶液A或溶液B中苯硼酸基团和步骤S3得到的多酚溶液中邻二醇基团的摩尔比为2~6:1。
本发明所述的多酚交联天然多糖基水凝胶敷料，其特征在于是基于上述方法制得的。
本发明所述的多酚交联天然多糖基水凝胶敷料在制备生物医用敷料中的应用。
本发明与现有技术相比具有以下优点和有益效果：本发明提供的具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料包含生物相容性良好的天然多糖和提供多功能性的天然多酚，避免了传统水凝胶敷料通过负载抗菌、抗炎药物实现多功能的耐药性等缺点，具有优异的促进创面愈合的作用。
附图说明
图1是本发明实施例3制备的水凝胶敷料冻干后的扫描电子显微镜图；
图2是本发明实施例3制备的水凝胶敷料的抗菌性能测试结果；
图3是本发明实施例3制备的水凝胶敷料的抗氧化性测试结果；
图4是本发明实施例3制备的水凝胶敷料在小鼠皮肤全层伤口实验第14天时伤口组织的HE染色图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
步骤S1：将0.25g羟乙基壳聚糖溶于5mL去离子水中得到羧甲基壳聚糖溶液；
步骤S2： 将4.5mg 4-甲酰基苯硼酸加入到步骤S1所得溶液中室温下搅拌至全部溶解；
步骤S3：将50mg原花青素溶于5mL去离子水中得到原花青素溶液；
步骤S4：将步骤S2得到的溶液与步骤S3得到溶液等体积混匀，于室温下静置180min得到具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料。
实施例2
步骤S1：将0.32g醛基透明质酸钠溶于4mL去离子水中得到醛基透明质酸钠溶液；
步骤S2：将4mg 3-氨基苯硼酸加入到步骤S1所得溶液中室温下搅拌至全部溶解；
步骤S3：将60mg表没食子儿茶素没食子酸酯溶于4mL去离子水中得到表没食子儿茶素没食子酸酯溶液；
步骤S4：将步骤S2得到的溶液与步骤S3得到溶液按照体积比1:0.8混匀，于室温下静置300min得到具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料。
实施例3
步骤S1：将0.3g羧甲基基壳聚糖溶于5mL去离子水中得到羧甲基壳聚糖溶液；
步骤S2：将5mg 4-甲酰基苯硼酸加入到步骤S1所得溶液中室温下搅拌至全部溶解；
步骤S3：将0.15g单宁酸溶于5mL去离子水中得到单宁酸溶液；
步骤S4：将步骤S2得到的溶液与步骤S3得到溶液按照体积比1:1.2混匀，于室温下静置30min得到具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料。
为了说明本发明提供的具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料的各项性能，对实施例3制备的具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料进行测试，测试结果见图1～4。
图1为实施例3制备的水凝胶敷料冻干后的扫描电子显微镜图，可以观察到三维网状凝胶骨架结构。
图2为实施例3制备的水凝胶敷料的抗菌性能测试结果，如图所示，相对于空白对照组，制备的多功能水凝胶敷料对革兰氏阴性的大肠杆菌和革兰氏阳性的金黄色葡萄球菌展现出优异的抗菌性能。
图3为实施例3制备的水凝胶敷料的抗氧化性测试结果，如图所示，制备的多功能水凝胶敷料对ABTS+自由基展现出良好的清除能力。
图4为实施例3制备的水凝胶敷料在小鼠皮肤全层伤口实验第14天时伤口组织的HE染色图，相对于空白对照组，制备的多功能水凝胶敷料组具有较多的毛孔、血管等较为完整的皮肤组织和附属器官，证明了所制备多功能水凝胶敷料具有良好的促进伤口愈合的性能。
综上，本发明提供的具有内在抗菌、抗氧化、促愈合等多功能性的水凝胶敷料展现出良好的抗菌、抗氧化等性能，并在小鼠皮肤全层伤口实验中，能够促进较为完整的皮肤组织及其附属器官从而加速伤口的愈合。
以上显示和描述了本发明的基本原理、主要特征和优点，在不脱离本发明精神和范围的前提下，本发明还有各种变化和改进，这些变化和改进都要求落入本发明的保护范围之内。
Claims (9)
1.一种多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于具体步骤为：
步骤S1：将含有氨基的天然多糖或含有醛基的天然多糖溶于去离子水中得到氨基多糖溶液或醛基多糖溶液，其中含有氨基的天然多糖为壳聚糖、羧甲基壳聚糖、羧乙基壳聚糖或羟乙基壳聚糖中的一种或多种；
步骤S2：将3-甲酰基苯硼酸或4-甲酰基苯硼酸加入到步骤S1得到的氨基多糖溶液中并于室温搅拌至全部溶解得到溶液A，或者将3-氨基苯硼酸或4-氨基苯硼酸加入到步骤S1得到的醛基多糖溶液中并于室温搅拌至全部溶解得到溶液B；
步骤S3：将天然多酚溶于去离子水中得到多酚溶液，其中天然多酚为原花青素、表没食子儿茶素没食子酸酯、表没食子儿茶素、表儿茶酚没食子酸、单宁酸、鞣花酸、芦丁或棉酚中的一种或多种；
步骤S4：将步骤S2得到的溶液A或溶液B与步骤S3得到的多酚溶液混匀，再于室温静置即可得到具有内在抗菌、抗氧化、促愈合功能性的多酚交联天然多糖基水凝胶敷料。
2.根据权利要求1所述的多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于步骤S1中所述含有醛基的天然多糖的具体制备过程为：
步骤S101：将含有邻二醇结构的天然多糖溶于去离子水中得到含有邻二醇结构的天然多糖溶液，其中含有邻二醇结构的天然多糖为海藻酸钠、透明质酸钠、魔芋胶、瓜尔豆胶、阿拉伯树胶、葡聚糖、纤维素、硫酸软骨素或肝素中的一种或多种；
步骤S102：将高碘酸钠溶于去离子水中得到高碘酸钠溶液；
步骤S103：将步骤S102得到的高碘酸钠溶液加入到步骤S101得到的含有邻二醇结构的天然多糖溶液中混匀，于室温下避光搅拌反应，再向反应液中加入乙二醇继续反应，反应完成后将反应液装入透析袋，放入去离子水中透析后冻干得到含有醛基的天然多糖。
3.根据权利要求2所述的多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于：步骤S103中所述高碘酸钠与含有邻二醇结构的天然多糖的摩尔比为0.2~2:1。
4.根据权利要求1所述的多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于：步骤S1中所述氨基多糖溶液或醛基多糖溶液的浓度为2~150mg/mL。
5.根据权利要求1所述的多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于：步骤S2中所述3-甲酰基苯硼酸或4-甲酰基苯硼酸与氨基多糖溶液中氨基的摩尔比为0.05~0.2:1，3-氨基苯硼酸或4-氨基苯硼酸与醛基多糖溶液中醛基的摩尔比为0.05~0.4:1。
6.根据权利要求1所述的多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于：步骤S3中所述多酚溶液的浓度为5~100mg/mL。
7.根据权利要求1所述的多酚交联天然多糖基水凝胶敷料的制备方法，其特征在于步骤S4中所述溶液A或溶液B与多酚溶液的投料配比满足：步骤S2得到的溶液A或溶液B中苯硼酸基团和步骤S3得到的多酚溶液中邻二醇基团的摩尔比为2~6:1。
8.一种多酚交联天然多糖基水凝胶敷料，其特征在于是基于权利要求1~7中任意一项所述的方法制得的。
9.权利要求8所述的多酚交联天然多糖基水凝胶敷料在制备生物医用敷料中的应用。
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