CN113975451A - 一种自愈合抗菌组织粘附水凝胶及其制备方法和用途 - Google Patents

一种自愈合抗菌组织粘附水凝胶及其制备方法和用途 Download PDF

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CN113975451A
CN113975451A CN202111268527.9A CN202111268527A CN113975451A CN 113975451 A CN113975451 A CN 113975451A CN 202111268527 A CN202111268527 A CN 202111268527A CN 113975451 A CN113975451 A CN 113975451A
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蒋玉仁
杨顺
杨婷婷
韩婷
熊芳姣
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Abstract

本发明公开了一种自愈合抗菌组织粘附水凝胶材料及其制备方法和用途。本发明以壳聚糖为原料，表面引入邻苯三酚基团，利用银离子与邻苯三酚基团的配位作用以及壳聚糖的羟基、邻苯三酚基团与聚丙烯酸的羧基之间形成氢键生成双交联水凝胶材料。所述的水凝胶组分有含羟基高分子、单宁酸、硝酸银、丙烯酸、过硫化物及交联剂，将它们混合后在室温下充分聚合，得到水凝胶材料。其中含羟基高分子与邻苯三酚之间形成氢键，邻苯三酚与银离子之间的氧化还原系统催化丙烯酸在交联剂和过硫化物的作用下聚合形成共聚物，同时聚丙烯酸的羧基能够与含羟基的高分子、邻苯三酚之间形成氢键，使得水凝胶具有较高的交联密度。该水凝胶组织粘附强度高，剪切强度大，制备条件简单。

Description

一种自愈合抗菌组织粘附水凝胶及其制备方法和用途
技术领域
本发明涉及一种自愈合抗菌组织粘附水凝胶及其制备方法和用途，属于功能高分子材料领域。
背景技术
创伤或手术损伤后伤口的闭合和修复具有重要的临床和研究意义。针对于人体组织伤口闭合处理，缝合线仍然是常见的伤口闭合技术，但是这类方法操作繁琐，还可能会因伤口密封不严造成感染等缺点。因此，聚合物水凝胶粘合剂因其可调节的化学和物理特性而成为伤口处理和修复的合适材料，它们能够粘附或粘附于组织，具有足够的机械强度以保持完好无损并随后被去除，提供完全的伤口闭合，并成为细菌感染的屏障。此外，这些材料吸收伤口渗出液并保持伤口湿润，以加快愈合速度。
壳聚糖、海藻酸钠、胶原蛋白等都是天然高分子材料，具有良好的生物相容性以及抗菌作用，是人体组织工程中的常用材料。但由于单独使用这类天然高分子材料，将其作为水凝胶的主要成分，其粘合能力往往达不到人们的期望。如在申请号为201510891554.X的发明专利中，公开了一种医用粘合剂及其制备方法，制备方法是将等体积的浓度为10％～50％(w/v)的醛基化海藻酸钠溶液与1％～6％(w/v)的氨基化羧甲基壳聚糖溶液混合，席夫碱反应形成水凝胶，其水凝胶的猪皮粘接强度为10～30gfcm-2，粘附强度不够突出。
在公开号为CN 110947027 B的发明专利中，公开了一种抑菌型促进创面修复的自愈合水凝胶敷料，所述的一种抑菌型促进创面修复的自愈合水凝胶敷料制备方法是将胶原蛋白配成溶液，将苯甲醛封端的聚乙二醇聚合物溶于胶原蛋白溶液中配置成混合液，并在混合液覆盖8-15mL多巴胺溶液，静置一定时间后去除，反复润洗2～3次水凝胶，制得具有抑菌功能的水凝胶敷料，其中，胶原蛋白和醛基化修饰的聚乙二醇聚合物的质量比为(2～4):(0.3～21.2)。此发明所述的以胶原蛋白和苯甲醛封端的聚乙二醇为水凝胶基质，通过原位聚合的方式修饰以聚多巴胺，改性聚乙二醇聚合物的醛基、聚多巴胺与组织的化学作用及胶原蛋白的静电作用、疏水作用，这些作用使共同使水凝胶具有一定的粘附性能。但此水凝胶的粘附强度为5kPa～6.16kPa，存在粘附能力不足的缺点。另外，在制备苯甲醛封端的聚乙二醇组分时用到的对醛基苯甲酸及四氢呋喃等都是有毒有害物质，因此在实际运用过程中很容易因纯化不彻底而对生物造成毒害作用。
因此临床上需要一种组织粘附性能强，制备简单，成本低廉，操作方便快捷，具有自愈合功能同时能有效抗菌的组织粘附水凝胶。
发明内容
本发明的目的是提供一种组织粘附性能强，制备简单，成本低廉，操作方便快捷，具有自愈合功能同时能有效抗菌的组织粘附水凝胶。
本发明的另一目的在于提供上述自愈合抗菌组织粘附水凝胶的制备方法。
本发明的技术方案如下：
所述的自愈合抗菌组织粘附水凝胶，由包括如下质量比的组分制成：壳聚糖:单宁酸:硝酸银:丙烯酸单体:去离子水:交联剂:过硫化物＝(30～150):(10～50):(20～110):10:(10～20):(10～20):(70～80)。
其中，过硫化物作为引发剂，浓度为0.02g/mL，交联剂为浓度为0.01g/mL的N,N'-亚甲基双丙烯酰胺溶液。
所述过硫化物包括过硫酸铵和过硫酸钾。
所述自愈合抗菌组织粘附水凝胶的制备方法，包括如下步骤：
(1)壳聚糖-单宁酸-纳米银溶液的制备：
将壳聚糖溶于体积分数为2％的冰醋酸溶液中，得到壳聚糖溶液，所述壳聚糖溶液中壳聚糖质量分数为2％。接着加入单宁酸室温搅拌反应4h，再加入硝酸银固体，室温避光反应30min，得到壳聚糖-单宁酸-纳米银溶液，制得溶液1。
(2)丙烯酸溶液的制备：
取丙烯酸单体，依次加入交联剂、过硫化物、去离子水，搅拌均匀，制得溶液2。
(3)自愈合抗菌组织粘附水凝胶的制备：
将步骤(1)所得的溶液1加入到步骤(2)所得的溶液2中，混合均匀，即得均匀的混合物；然后将所得的混合物在室温下吸取至聚四氟乙烯模具中进行自聚合，即得所述自愈合抗菌组织粘附水凝胶。
与现有技术相比，本发明的优点有：(1)本发明的壳聚糖-单宁酸-纳米银自愈合组织粘附水凝胶材料所选用的原料为壳聚糖、丙烯酸二者都具有毒性低、安全性相对较高等优点，且壳聚糖和银离子具有一定抗菌作用；(2)本发明制备的壳聚糖-单宁酸-纳米银自愈合水凝胶材料利用羟基与邻苯三酚、羧基之间形成大量氢键，使得水凝胶具有多维度，高交联密度的交联方式，使水凝胶具有较高的机械强度与粘附强度，能提供自愈合性和长期、可重复粘合性；(3)本发明的自愈合组织粘附水凝胶组分包括壳聚糖和银，两者均能有效抑制革兰氏阳性细菌和金黄色葡萄球菌；(4)本发明的组织粘附水凝胶，原料廉价易得，制作简单且周期短，愈合条件简单、愈合效果好，在用于创面时可直接使用。
附图说明
图1为本发明实施例3所制备的自愈合组织粘附水凝胶的实物照片，从左至右依次为：剪切前、剪切后、自愈合后的照片。
图2为空白样、本发明实施例1、实施例3和对比例1所制备的自愈合组织粘附水凝胶抑制大肠杆菌和金黄色葡萄球菌的照片。A1-A4依次为空白样、对比例1、本发明实施例1和实施例3所制备的水凝胶对大肠杆菌抑制效果；B1-B4依次为空白样、对比例1、本发明实施例1和实施例3所制备的水凝胶对金黄色葡萄球菌抑制效果。
具体实施方式
以下结合具体实施例对本发明的技术方案作进一步说明，但这些实施例并不对本发明做任何形式的限定。实施例中若无特别说明，则都为常规试剂与常规方法。
实施例1
将10mg壳聚糖(相对分子质量为10000～200000)溶解于0.5mL体积分数为2％冰醋酸溶液中，溶解后加入3.4mg单宁酸室温搅拌反应4h，再加入7.5mg硝酸银避光反应30min得溶液1；另取2.7mL的丙烯酸溶液，加入1mL过硫化物溶液(浓度为0.02g/mL)，加入300μL的交联剂(浓度为0.01g/mL)以及4mL去离子水混合均匀得溶液2；将溶液1加入至溶液2中，混合均匀，将此混合液置于模具中，室温下聚合8min，即得到一种自愈合组织粘附水凝胶。
实施例2
将20mg壳聚糖(相对分子质量为10000～200000)溶解于1mL体积分数为2％冰醋酸溶液中，溶解后加入6.7mg单宁酸室温下搅拌反应4h，再加入15mg硝酸银避光反应30min得溶液1；另取2.7mL的丙烯酸溶液，加入1mL过硫化物溶液(浓度为0.02g/mL)，加入300μL的交联剂(浓度为0.01g/mL)以及4mL去离子水混合均匀得溶液2；将溶液1加入至溶液2中，混合均匀，将此混合液置于模具中，室温下聚合8min，即得到一种自愈合组织粘附水凝胶。
实施例3
将30mg壳聚糖(相对分子质量为10000～200000)溶解于1.5mL体积分数为2％冰醋酸溶液中，溶解后加入10.1mg单宁酸室温搅拌反应4h，再加入22.5mg硝酸银避光反应30min得溶液1；另取2.7mL的丙烯酸溶液，加入1mL过硫化物溶液(浓度为0.02g/mL)，加入300μL的交联剂(浓度为0.01g/mL)以及4mL去离子水混合均匀得溶液2；将溶液1加入至溶液2中，混合均匀，将此混合液置于模具中，室温下聚合6min，即得到一种自愈合组织粘附水凝胶。
实施例4
将40mg壳聚糖(相对分子质量为10000～200000)溶解于2mL体积分数为2％冰醋酸溶液中，溶解后加入13.4mg单宁酸室温搅拌反应4h，再加入30mg硝酸银避光反应30min得溶液1；另取2.7mL的丙烯酸溶液，加入1mL过硫化物溶液(浓度为0.02g/mL)，加入300μL的交联剂(浓度为0.01g/mL)以及4mL去离子水混合均匀得溶液2；将溶液1加入至溶液2中，混合均匀，将此混合液置于模具中，室温下聚合8min，即得到一种自愈合组织粘附水凝胶。
对比例1
首先将丙烯酸溶液(2.7mL)、交联剂(300μL，0.01gmL-1)、四甲基乙二胺(30μL)、过硫化物(1mL，0.02gmL-1)和去离子水(6mL)放入烧杯搅拌，制成均一溶液。然后将样品置于60℃的氮气气氛中30min，以获得PAA水凝胶。
性能测试
将上述实施例1-4、对比例1所制得的水凝胶分别施于猪皮表面，施胶面积为15mm×15mm，施胶厚度为1mm，两块猪皮粘合后用手按压30s，然后用万能试验机进行剪切强度测试，测试的剪切强度结果如下表。
实验例 剪切强度
实施例1 13.85kPa
实施例2 15.78kPa
实施例3 20.10kPa
实施例4 15.67kPa
对比例1 7.88kPa
抗菌测试
将无菌水、上述对比例1、实施例1和实施例3所制得的水凝胶各取0.2g，加入含有5mL大肠杆菌(ATCC25922)或金黄色葡萄球菌(ATCC25923)溶液(1×106CFU mL-1)的离心管中，在37℃、110r/min下振荡4-6h。取50μL溶液稀释100倍，吸取100μL菌液均匀铺于营养琼脂培养皿上共培养6-8h，观察各培养皿中菌落数。图2为空白样、本发明实施例1、实施例3和对比例1所制备的自愈合组织粘附水凝胶抑制大肠杆菌和金黄色葡萄球菌的效果。其中，A1-A4依次为空白样、对比例1、本发明实施例1和实施例3所制备的水凝胶对大肠杆菌抑制效果，B1-B4依次为空白样、对比例1、本发明实施例1和实施例3所制备的水凝胶对金黄色葡萄球菌抑制效果。结果显示，空白样、对比例1对大肠杆菌和金黄色葡萄球菌无抑菌作用，而本发明实施例1、实施例3对大肠杆菌和金黄色葡萄球菌均具有明显抑菌效果。

Claims (4)

1.一种壳聚糖-单宁酸-纳米银自愈合抗菌水凝胶材料，其特征在于：由包括如下质量比的组分制成：壳聚糖:单宁酸:硝酸银:丙烯酸单体:去离子水:交联剂:过硫化物＝(30～150):(10～50):(20～110):10:(10～20):(10～20):(70～80)；
其中，过硫化物作为引发剂，浓度为0.02g/mL；交联剂是浓度为0.01g/mL的N,N'-亚甲基双丙烯酰胺溶液；
其制备方法包括如下步骤：
(1)壳聚糖-单宁酸-纳米银溶液的制备：
将壳聚糖溶于体积分数为2％的冰醋酸溶液中，得到壳聚糖溶液，所述壳聚糖溶液质量分数为2％。接着加入单宁酸，室温搅拌反应4h。再加入硝酸银固体，室温避光反应30min，得到壳聚糖-单宁酸-纳米银溶液，制得溶液1；
(2)丙烯酸溶液的制备：
取丙烯酸单体，依次加入交联剂、过硫化物、去离子水，搅拌均匀，制得溶液2；
(3)自愈合抗菌组织粘附水凝胶的制备：
将步骤(1)所得的溶液1加入到步骤(2)所得的溶液2中，混合均匀，然后在室温下吸取混合溶液至聚四氟乙烯模具中进行自聚合，即得所述自愈合抗菌组织粘附水凝胶。
2.权利要求1所述的一种自愈合水凝胶，其特征在于：所述的步骤(1)中所述壳聚糖的分子量为10000～200000。
3.权利要求1所述的一种自愈合水凝胶，其特征在于：所述过硫化物包括过硫酸铵和过硫酸钾。
4.权利要求1所述一种自愈合抗菌组织粘附水凝胶在制备医用粘合剂中的应用。
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