CN110117369B - 一种抗菌粘附的导电水凝胶及其制备方法和应用 - Google Patents

一种抗菌粘附的导电水凝胶及其制备方法和应用 Download PDF

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CN110117369B
CN110117369B CN201910405038.XA CN201910405038A CN110117369B CN 110117369 B CN110117369 B CN 110117369B CN 201910405038 A CN201910405038 A CN 201910405038A CN 110117369 B CN110117369 B CN 110117369B
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林权
赵月
刘厚
赵玥琪
杨喆
杨柏
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Abstract

一种抗菌粘附的导电水凝胶及其制备方法和应用属于功能高分子材料技术领域。本发明采用将合成的聚多巴胺修饰的银纳米粒子，复合在导电聚合物单体以及聚乙烯醇的溶液中，利用引发剂引发聚合，原位制备导电功能水凝胶。该水凝胶具有良好的生物相容性，高的生物粘附性，优良的导电性质，以及对于革兰氏阴性菌和革兰氏阳性菌的优良抗菌性能，力学性质可以调节。可以作为一种新型医用高分子伤口敷料，在促进肌体伤口愈合等方面具有潜在的生物和医学应用价值。

Description

一种抗菌粘附的导电水凝胶及其制备方法和应用
技术领域
本发明属于高分子材料技术领域，具体涉及一种抗菌粘附的导电水凝胶、制备方法及其在伤口敷料上的应用。
背景技术
皮肤是人体最大的器官，具有保护人体免受损伤，防止微生物入侵，维持体液和电解质平衡等作用。一旦皮肤出现严重缺陷，伤口将严重影响人们的生活和健康。伤口，特别是广泛的全厚伤口，需要很长时间才能修复，而急慢性伤口一直是临床的主要问题。因此，开发具有快速闭合伤口、促进伤口愈合和防止细菌滋生等特点的伤口敷料具重要的临床价值。迄今为止，多种生物材料包括静电纺丝纳米纤维、多孔泡沫、高分子膜和功能性水凝胶等，已被用于促进伤口愈合的敷料。在所有生物材料中，水凝胶敷料因其具有维持湿润的伤口环境，吸收组织渗出物，允许氧气渗透和冷却伤口表面，从而减轻患者的疼痛等特点，而备受瞩目。
尽管最近开发的基于水凝胶的伤口敷料，在一定程度上促进了伤口的愈合，但是这些传统的水凝胶容易吸收微生物，并且容易受大量寄生在人体皮肤表面的病原菌感染，从而引发炎症反应、伤口感染或免疫反应，对人体健康构成直接威胁。此外，皮肤也是一种电信号敏感组织，具有2.6mS/cm到1×104mS/cm的传导率。电活性材料已被证明可以有效地促进细胞的粘附、增殖、迁移等。因此，开发具有抗菌性粘附导电水凝胶能够进一步地促进伤口愈合，在临床上具有重要的意义。
发明内容
本发明的目的是提供一种抗菌粘附的导电水凝胶、制备方法及其在伤口敷料上的应用。
该方法首先合成了聚多巴胺修饰的银纳米粒子；然后在90℃下将导电聚合物单体以及聚乙烯醇加入到上述溶液中，利用引发剂引发聚合，形成深绿色的导电水凝胶。该水凝胶具有良好的生物相容性，粘附性，以及抗菌性能。综合以上优异的性质，该抗菌粘附电活性水凝胶作为一种新型医用高分子伤口敷料，在促进了体内伤口愈合方面具有潜在的生物和医学应用价值。
本发明所述的具有抗菌粘附的导电水凝胶的制备方法，其具体步骤如下：
(1)首先，将硝酸银(0.1mM，10～100mL)、柠檬酸钠(180mm，1～10mL)、聚乙烯吡咯烷酮(4.2mM,1～10mL)和过氧化氢(30wt.％，0.24～0.5mL)的水溶液混合，并在室温下敞口剧烈搅拌。然后将硼氢化钠(100mm，0.60～1.0mL)快速加入以上混合溶液中。反应30分钟后，获得银纳米粒子的胶体溶液。
(2)将反应物1(47.5～285mg)溶解于以上制备的银纳米粒子水溶液中。通过滴加NaOH溶液(1M)，将体系的pH调整到8.5～11，并在室温下敞口剧烈搅拌2个小时即可得到反应物1包覆的银纳米粒子。
(3)抗菌粘附导电水凝胶的制备。取上述制备的反应物1包覆的银纳米粒子溶液(9～45mL)，加入反应物2(1～5g)，90℃下搅拌直至完全溶解。然后加入苯胺(100～500μL)，3-氨基苯基硼酸(75～375mg)，反应物3(835～4175μL，6M)继续搅拌2个小时。冷却到室温后，加入反应物4溶液(808～4040μL,6M)后，形成深绿色的力学性质弱的导电水凝胶。最后，将上述制备的导电水凝胶在-40℃冷却过夜。最终得到力学性能大范围可调的抗菌粘附导电水凝胶。
上述方法中，银纳米粒子可以是三角形、球形等。
上述方法中，反应物1可以是单宁酸、多巴胺、没食子酸等。
上述方法中，反应物2可以是聚乙烯醇、明胶、琼脂、壳聚糖、纤维素等。
上述方法中，反应物3可以是盐酸、硝酸、硫酸。
上述方法中，反应物4可以是过硫酸铵、过硫酸钾。
本发明具有如下优点：1.所制得的水凝胶可以通过改变组分的含量改变其力学性质，进而获得大范围可调的机械性能。从低模量到高的模量，增加了水凝胶在实际应用中的界面的稳定性和环境适应性，进而极大地拓展了水凝胶材料在生物医用材料方面的应用前景。2.所制备的导电水凝胶以聚苯胺和生物相容性好的聚合物为主要原料，赋予了水凝胶良好的导电性，并且具有无毒，价廉，生物相容性好等特点。3.不同传统的导电水凝胶，该导电水凝胶对革兰氏阴性(大肠杆菌)和革兰氏阳性(金黄色葡萄球菌)都具有明显的抑制效果，即该水凝胶具有广谱的抗菌活性。4.该水凝胶含水量高，可以达到90％以上。冻干后的电镜图可以证明该水凝胶为疏松多孔状，这样的结构有利于气体的运输，物质的交换等。5.由于水凝胶的成胶时间是可以调节，因此该水凝胶具有良好的加工性质，可以利用3D打印、塑模、注射等方式，形成各种形状，以满足其实际需要。
附图说明
图1：为实施例1制备的抗菌导电水凝胶的相态变化图。通过试剂瓶倾斜实验可以看出，制备的多巴胺包覆的银纳米粒子、苯胺、3-氨基苯基硼酸、聚乙烯醇的混合溶液在室温下呈溶胶态，加入过硫酸铵之后，从溶胶变成凝胶。
图2：为实施例1制备的抗菌导电水凝胶的电镜图。由图可知，该水凝胶为疏松多孔状。
图3：为实施例1制备的抗菌导电水凝胶的抗菌效果图。随着水凝胶中的银纳米粒子的增多，琼脂板上的抗菌环的面积越来越大，说明导电水凝胶的抗菌效果增强。
图4：为实施例1制备的抗菌导电水凝胶和对照组对糖尿病足伤口治疗的效果图。与对照组相比，抗菌导电水凝胶作为伤口敷料可以有效地促进糖尿病足伤口的愈合，具有更快的创面愈合率。
具体实施方式
实施例1：
(1)将硝酸银(0.1mM，97mL)、柠檬酸钠(180mm，1mL)、聚乙烯吡咯烷酮(4.2mM,1mL)和过氧化氢(30wt.％，0.24mL)的溶液混合，并在室温下敞口剧烈搅拌。然后将硼氢化钠(100mm，0.30mL)快速加入以上混合溶液中。反应30分钟后，获得形状为三角形的银纳米粒子的蓝色胶体溶液。
(2)多巴胺95mg溶解于以上制备的银纳米粒子水溶液中。通过滴加NaOH溶液(1M)，将体系的pH调整到8.5，并在室温下敞口剧烈搅拌2个小时即可得到多巴胺包覆的银纳米粒子。
(3)抗菌粘附导电水凝胶的制备。取上述制备的多巴胺包覆的银纳米粒子溶液9mL，加入聚乙烯醇1g，90℃下搅拌直至完全溶解。然后加入苯胺200μL，3-氨基苯基硼酸75mg，盐酸(1000μL，6M)继续搅拌2个小时。冷却到室温后，加入过硫酸铵溶液(808μL,6M)后，形成深绿色的力学性质弱的导电水凝胶。最后，将上述制备的导电水凝胶在-40℃冷却过夜。最终得到力学性能大范围可调的抗菌粘附导电水凝胶。
实施例2：
(1)将硝酸银(0.1mM，97mL)、柠檬酸钠(180mm，1mL)、聚乙烯吡咯烷酮(4.2mM,1mL)和过氧化氢(30wt.％，0.24mL)的溶液混合，并在室温下敞口剧烈搅拌。然后将硼氢化钠(100mm，0.30mL)快速加入以上混合溶液中。反应30分钟后，获得形状为三角形的银纳米粒子的蓝色胶体溶液。
(2)单宁酸95mg溶解于以上制备的银纳米粒子水溶液中。通过滴加NaOH溶液(1M)，将体系的pH调整到8.5，并在室温下敞口剧烈搅拌2个小时即可得到单宁酸包覆的银纳米粒子。
(3)抗菌粘附导电水凝胶的制备。取上述制备的单宁酸包覆的银纳米粒子溶液9mL，加入琼脂1g，90℃下搅拌直至完全溶解。然后加入苯胺200μL，3-氨基苯基硼酸75mg，硫酸(1000μL，6M)继续搅拌2个小时。冷却到室温后，加入过硫酸钾溶液(808μL,6M)后，形成深绿色的力学性质弱的导电水凝胶。最后，将上述制备的导电水凝胶在-40℃冷却过夜。最终得到力学性能大范围可调的抗菌粘附导电水凝胶。

Claims (4)

1.一种抗菌粘附的导电水凝胶的制备方法，其特征在于：具体步骤如下：
（1）首先，将0.1 mM硝酸银10~100 mL、180 mM柠檬酸钠1~10 mL、4.2 mM聚乙烯吡咯烷酮 1~10 mL和30 wt.%过氧化氢0.24~0.5 mL的水溶液混合，并在室温下敞口剧烈搅拌；然后将100 mM硼氢化钠0.60~1.0 mL快速加入以上混合溶液中；反应30分钟后，获得银纳米粒子的胶体溶液；
（2）将47.5~285 mg反应物1 溶解于以上制备的银纳米粒子水溶液中；通过滴加1 MNaOH溶液，将体系的pH调整到8.5~11，并在室温下敞口剧烈搅拌2个小时即可得到反应物1包覆的银纳米粒子；所述的反应物1为单宁酸、多巴胺或没食子酸；
（3）抗菌粘附导电水凝胶的制备；取上述制备的反应物1包覆的银纳米粒子溶液9~45mL，加入1~5 g反应物2，90 ℃下搅拌直至完全溶解；然后加入苯胺100~500 μL，3-氨基苯基硼酸75~375 mg，6 M反应物3 835~4175 μL，继续搅拌2个小时，反应物3为盐酸、硝酸或硫酸；冷却到室温后，加入6 M反应物4溶液808~4040 μL后，形成深绿色的力学性质弱的导电水凝胶，反应物4为过硫酸铵或过硫酸钾；最后，将上述制备的导电水凝胶在-40ºC冷却过夜；最终得到力学性能大范围可调的抗菌粘附导电水凝胶；所述的反应物2为聚乙烯醇、明胶、琼脂、壳聚糖或纤维素。
2.根据权利要求1所述的一种抗菌粘附的导电水凝胶的制备方法，其特征在于：步骤（1）中所述的银纳米粒子是三角形或球形。
3.根据权利要求1-2所述的任一种抗菌粘附的导电水凝胶的制备方法所制得的导电水凝胶。
4.根据权利要求3所述的一种导电水凝胶在制备伤口敷料上的应用。
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