CN113750285A - 一种复合气凝胶敷料及其制备方法 - Google Patents
一种复合气凝胶敷料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种复合气凝胶敷料及其制备方法。本发明的一种复合气凝胶敷料，该气凝胶敷料由下述质量百分比的原料组成：聚乙烯醇4％～10％、水溶性壳聚糖5％～50％、氧化石墨烯0.1％～3％，余量为去离子水。一种如上述的复合气凝胶敷料的制备方法，按照上述质量百分比配置混合溶液，将混合溶液先冷冻再解冻多次得水凝胶，将得到的水凝胶冷冻干燥得复合气凝胶敷料。本发明的复合气凝胶敷料具有止血、抗菌和促进伤口愈合的功能，同时成本低、环保、制备工艺简单、对设备没有特殊要求和较好的生物相容性，在医用伤口敷料方面具有很大的潜能。
Description
技术领域
本发明涉及医用材料技术领域，尤其涉及一种复合气凝胶敷料及其制备方法。
背景技术
传统的医用敷料，如医用棉球、纱布或绷带等，都能在不同程度上吸收伤口渗出液，而且对伤口也有一定的保护作用，但这类伤口敷料只能是暂时性的覆盖材料，传统的医用伤口敷料通常是干燥的，不能为伤口提供湿润的愈合环境，当敷料被浸湿后，极易引发伤口的外源性感染。另外，传统的伤口敷料在换药时很容易与伤口发生粘结，造成二次伤害，延迟创面的愈合过程。与传统伤口敷料相比，新型医用敷料不仅能更好的覆盖伤口表面，还能提供合适的愈合环境，加速伤口组织的再功能化和修复过程。理想的新型伤口敷料一般应该有以下功能：能够吸收过多的组织渗出液，同时避免水分和体液的过分散失；透湿、透气且能为伤口维持湿润的环境；能够抵御外界微生物的入侵，控制伤口的感染；换药时更换容易，不会引起皮肤伤口的二次损害。根据原料来源，新型医用敷料一般可以分为合成高分子材料类和天然高分子材料类，包括海绵、凝胶、泡沫和薄膜等。但是在新型医用敷料中例如泡沫、海绵和薄膜也存在一定的缺陷。泡沫敷料吸收渗液后敷料局部会变为白色,可能造成误会。粘性较大,如果使用较短时间就去除,敷料粘性仍然很大时可能造成皮肤损伤；海绵敷料可能需要使用二层敷料或胶带固定；渗液较多时，如果没有及时更换，可能会引起伤口周围皮肤浸渍，在更换时不易移除，会对伤口造成二次伤害；周围皮肤脆弱或感染伤口时不能使用薄膜敷料。
发明内容
本发明的目的在于，针对现有技术的上述不足，提出一种具有止血、抗菌和促进伤口愈合的功能的复合气凝胶敷料及其制备方法。
本发明的一种复合气凝胶敷料，该气凝胶敷料由下述质量百分比的原料组成：聚乙烯醇4％～10％、水溶性壳聚糖5％～50％、氧化石墨烯0.1％～3％，余量为去离子水。
进一步的，所述的聚乙烯醇的聚合度为1700，醇解度为99％。
进一步的，所述水溶性壳聚糖为水溶性羧甲基壳聚糖。
一种如上述的复合气凝胶敷料的制备方法，按照上述质量百分比配置混合溶液，将混合溶液先冷冻再解冻多次得水凝胶，将得到的水凝胶冷冻干燥得复合气凝胶敷料。
进一步的，所述的复合气凝胶敷料的具体制备步骤为：
(1)配制质量分数为4％～10％的聚乙烯醇水溶液，向聚乙烯醇水溶液中加入质量分数为5％～50％水溶性壳聚糖和质量分数为0.1％～3％的氧化石墨烯，室温下搅拌均匀后，静置脱泡；
(2)将(1)所得溶液倒入塑料培养皿中，在-18～-20度冷冻22～24h,室温下解冻2～4h，这个过程循环1～3次，得到水凝胶；
(3)将(2)所得水凝胶放入冷冻干燥机中冷冻干燥2～4天得复合气凝胶敷料。
本发明的复合气凝胶敷料包括氧化石墨烯、聚乙烯醇和壳聚糖，其中，氧化石墨烯是一种有前景的纳米材料，具有较大的表面积，在其表面有大量的羟基、羧基和环氧基团等官能团。氧化石墨烯具有各种实用性能，包括优异的化学稳定性、机械性能、生物相容性和亲水性等，添加氧化石墨烯可以改善材料的机械性质、生物活性和药物缓释性能而不会诱导细胞毒性，能促进细胞的生长增殖。
聚乙烯醇是一种水溶性的高分子聚合物，对人体是无毒无害的，具有良好的生物相容性、生物降解性和优异的机械性能。聚乙烯醇在反复冷冻解冻的情况下，聚乙烯醇分子间和分子内会形成氢键，进而形成具有三维网络结构的水凝胶，避免了有毒化学交联剂的使用，如戊二醛等。
水溶性羧甲基壳聚糖是壳聚糖的衍生物，具有快速愈合伤口并防止伤口感染的功能，水溶性好，并可减少对人体毒副作用。
本发明使用聚乙烯醇和水溶性壳聚糖为原料，充分的将两者的优点结合在一起，同时弥补各自的缺点，同步引入氧化石墨烯，制备出弹性柔韧性好、力学性能优异、具有止血抗菌促进伤口愈合的复合气凝胶敷料。
本发明气凝胶敷料的制备方法是冷冻解冻法、离子交联法和冷冻干燥法相结合。该制备方法操作简单、环保且制备出来的气凝胶敷料在吸收伤口渗液后从气凝胶变为水凝胶，水凝胶能抵御细菌的入侵，防止感染并与创面贴合良好；透湿、透气，并为创面愈合提供湿润的环境；不会在更换敷料时对伤口带来二次伤害。
冷冻解冻法使聚乙烯醇分子间和分子内通过氢键连接在一起，是物理交联，避免了有毒化学交联剂的使用，如硼酸、戊二醛等。
本发明的复合气凝胶敷料具有止血、抗菌和促进伤口愈合的功能，同时成本低、环保、制备工艺简单、对设备没有特殊要求和较好的生物相容性，在医用伤口敷料方面具有很大的潜能。
附图说明
图1是实施例2所得复合气凝胶的扫描截面图。
具体实施方式
以下是本发明的具体实施例并结合附图，对本发明的技术方案作进一步的描述，但本发明并不限于这些实施例。
实施例1：
(1)将PVA粉末加入到去离子水中，95℃加热搅拌2个小时，得到4wt％PVA水溶液。向4wt％PVA溶液中加入水溶性羧甲基壳聚糖(水溶性羧甲基壳聚糖占PVA质量的20％)，常温下搅拌一段时间，直至形成均匀的混合溶液。
(2)向(1)得到的PVA/CMCS混合液中加入GO(GO的质量占PVA质量的0.5％)，搅拌一段时间形成均匀的混合溶液，静置过夜除气泡。
(3)将(2)得到的GO/PVA/CMCS混合溶液倒入塑料培养皿中，-18℃冷冻22h,室温下解冻2h。冷冻解冻循环1次。
(4)将(3)得到的水凝胶放入冷冻干燥机中冷冻干燥3天，得到氧化石墨烯/聚乙烯醇/水溶性壳聚糖复合气凝胶敷料。
实施例2：
(1)将PVA粉末加入到去离子水中，95℃加热搅拌2个小时，得到4wt％PVA水溶液。向4wt％PVA溶液中加入水溶性羧甲基壳聚糖(水溶性羧甲基壳聚糖占PVA质量的25％)，常温下搅拌一段时间，直至形成均匀的混合溶液。
(2)向(1)得到的PVA/CMCS混合液中加入GO(GO的质量占PVA质量的1％)，搅拌一段时间形成均匀的混合溶液，静置过夜除气泡。
(3)将(2)得到的GO/PVA/CMCS混合溶液倒入塑料培养皿中，-18℃冷冻24h,室温下解冻4h。冷冻解冻循环2次。
(4)将(3)得到的水凝胶放入冷冻干燥机中冷冻干燥3天，得到氧化石墨烯/聚乙烯醇/水溶性壳聚糖复合气凝胶敷料。所得的复合气凝胶的扫描截面图如图1所示。
实施例3：
(1)将PVA粉末加入到去离子水中，95℃加热搅拌2个小时，得到4wt％PVA水溶液。向4wt％PVA溶液中加入水溶性羧甲基壳聚糖(水溶性羧甲基壳聚糖占PVA质量的30％)，常温下搅拌一段时间，直至形成均匀的混合溶液。
(2)向(1)得到的PVA/CMCS混合液中加入GO(GO的质量占PVA质量的1.5％)，搅拌一段时间形成均匀的混合溶液，静置过夜除气泡。
(3)将(2)得到的GO/PVA/CMCS混合溶液倒入塑料培养皿中，-18℃冷冻22h,室温下解冻4h。冷冻解冻循环3次。
(4)将(3)得到的水凝胶放入冷冻干燥机中冷冻干燥3天，得到氧化石墨烯/聚乙烯醇/水溶性壳聚糖复合气凝胶敷料。
对比例1：
和实施例2相比，在步骤(2)中未向PVA/CMCS混合溶液中加入氧化石墨烯，其余步骤与实施例2相同。
对比例2：
和实施例2相比，在步骤(2)中向GO/CMCS/PVA溶液中加入2％硼酸(占PVA质量)常温下搅拌形成均匀溶液。静置除气泡之后，直接倒入塑料培养皿中冷冻干燥3天。其余步骤和实施例2相同。
对比例3：
和实施例2相比，在步骤(2)中向GO/CMCS/PVA溶液中加入0.5％戊二醛(占PVA质量)常温下搅拌形成均匀溶液。静置除气泡之后，直接倒入塑料培养皿中冷冻干燥3天。其余步骤和实施例2相同。
选取实施例1～3和对比例1～3进行力学性能、止血性能和抑菌效果测试，止血性能采用溶血-凝血法进行测试，抑菌效果采用平板计数法进行测试，测试结果如下表所示。
以上未涉及之处，适用于现有技术。
虽然已经通过示例对本发明的一些特定实施例进行了详细说明，但是本领域的技术人员应该理解，以上示例仅是为了进行说明，而不是为了限制本发明的范围，本发明所属技术领域的技术人员可以对所描述的具体实施例来做出各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的方向或者超越所附权利要求书所定义的范围。本领域的技术人员应该理解，凡是依据本发明的技术实质对以上实施方式所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围。
Claims (5)
1.一种复合气凝胶敷料，其特征在于：该气凝胶敷料由下述质量百分比的原料组成：聚乙烯醇4％～10％、水溶性壳聚糖5％～50％、氧化石墨烯0.1％～3％，余量为去离子水。
2.如权利要求1所述的一种复合气凝胶敷料，其特征在于：所述的聚乙烯醇的聚合度为1700～2600，醇解度为90％～99％。
3.如权利要求2所述的一种复合气凝胶敷料，其特征在于：所述水溶性壳聚糖为水溶性羧甲基壳聚糖。
4.一种如权利要求1-3任一项所述的复合气凝胶敷料的制备方法，其特征在于：按照上述质量百分比配置混合溶液，将混合溶液先冷冻再解冻多次得水凝胶，将得到的水凝胶冷冻干燥得复合气凝胶敷料。
5.一种如权利要求4所述的复合气凝胶敷料的制备方法，其特征在于：所述的复合气凝胶敷料的具体制备步骤为：
(1)配制质量分数为4％～10％的聚乙烯醇水溶液，向聚乙烯醇水溶液中加入质量分数为5％～50％水溶性壳聚糖和质量分数为0.1％～3％的氧化石墨烯，室温下搅拌均匀后，静置脱泡；
(2)将(1)所得溶液倒入塑料培养皿中，在-18～-20度冷冻22～24h,室温下解冻2～4h，这个过程循环1～3次，得到水凝胶；
(3)将(2)所得水凝胶放入冷冻干燥机中冷冻干燥2～4天得复合气凝胶敷料。
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