CN113694244A - 一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料及其制备方法 - Google Patents

一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料及其制备方法 Download PDF

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CN113694244A
CN113694244A CN202111019756.7A CN202111019756A CN113694244A CN 113694244 A CN113694244 A CN 113694244A CN 202111019756 A CN202111019756 A CN 202111019756A CN 113694244 A CN113694244 A CN 113694244A
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高晶
袁香楠
张俊
王璐
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Donghua University
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Abstract

本发明公开了一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料及其制备方法。本发明的制备方法包括：(1)制备聚多巴胺改性氧化石墨烯；(2)在海藻酸钠水溶液中加入交联剂、聚多巴胺改性氧化石墨烯混合均匀，将棉纱布放置在该溶液中密封并静置，得到棉纱布增强水凝胶；(3)将(2)制备的水凝胶浸没于氯化铁溶液，随后在冰浴条件下浸于吡咯单体溶液中，最后得到棉纱布增强水凝胶导电敷料。该敷料具有良好的机械性能、光热抗菌性能、导电性能、吸水保湿性能、抗氧化活性和生物相容性，为伤口提供必要的力学支撑的同时，满足伤口愈合过程中对医用敷料的非抗生素光热抗菌、导电促愈合的功效要求，可用于易感染伤口的治疗和管理。

Description

一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料 及其制备方法
技术领域
本发明涉及一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料及其制备方法，属于生物医用纺织材料技术领域。
背景技术
皮肤是人体最大的器官，它可以调节体温，保护内部器官免受外部物理和化学物质侵害，为病原体和微生物提供物理屏障，并防止体液无节制流失。一旦受到创伤产生伤口，皮肤屏障会被破坏，皮肤正常生理功能受到影响。而伤口在愈合过程中，尤其是慢性伤口容易受到病原菌的感染，从而影响组织修复、延缓愈合过程。这些问题增加了伤口患者的痛苦和死亡率，而对于伤口的抗菌、促愈合治疗也大大加重了社会的医疗负担。
针对伤口愈合缓慢的问题，鉴于人体内部具有内源性生物电系统，研究者发现在伤口处施加生物电刺激和生物电池，或使用导电高分子等材料覆盖伤口等方式可有效促进伤口愈合。其中，导电高分子水凝胶兼具导电高分子优异的电学性能，可促进伤口细胞的迁移和伤口的愈合，以及水凝胶独特的吸水保湿性能，可为伤口提供有利于愈合的湿性环境，能紧密贴合却不粘连伤口，因此导电水凝胶十分适用于伤口敷料。目前研究的导电水凝胶材料有聚吡咯、聚苯胺和聚乙烯二氧噻吩等，其可与聚乙烯醇、明胶、海藻酸钠、羧甲基纤维素、聚丙烯酰胺等高分子形成互穿型网络水凝胶。但水凝胶敷料通常具有力学性能不佳的问题，作为敷料使用时需要进一步考虑增强其力学性能。
在目前使用的敷料中，棉纱布、棉绷带作为传统的纺织基材敷料使用最为广泛，并具有力学性能好、价格便宜、材料易得等优点，但其在伤口干燥时易与伤口粘连，且易被渗出物污染而感染伤口，不具有促进伤口愈合功效。基于导电水凝胶和传统棉纱布敷料各自的优势和存在的问题，可通过物理或化学方式将二者复合，发挥二者优势，制备具有良好导电性能、生物相容性、力学性能的医用敷料。现有改善水凝胶机械性能的方法包括添加纳米材料(CN109705406、CN 109054315)、设计双网络结构(CN 106589410、CN108721688)等，利用棉纱布增强水凝胶敷料的研究未见相关专利报道。
对于伤口感染问题，在当前所采用的抗菌方式中，抗生素使用最为广泛，但目前大量使用甚至滥用抗生素易导致细菌产生耐药性。光热抗菌法是通过光热剂可吸收能够到达人体深层内部的近红外光，并将光能转变为热能，通过高温破坏细菌的蛋白质达到抗菌的效果。这种方法具有避免细菌产生耐药性、抗菌广谱性、抗菌高效性和安全性等诸多优点。目前，光热剂在敷料中的研究主要包括光热消融肿瘤细胞、利用光热效应促进药物释放或/和协同抗生素、促愈合药物实现有效抗菌、促愈合等。专利CN 110384654在水凝胶中负载了硫化铜@多巴胺纳米粒子，利用光热性能和放疗作用治疗癌细胞，同时联合黄芪甲苷促进术后伤口愈合作用；专利CN 109276538公开了一种光热响应载药水凝胶的设计合成方法，基于光照情况下硫化铜可产生热能促使水凝胶中药物分子快速扩散释放到作用位点；专利CN111773429在水凝胶敷料网状结构内搭载二硫化钨光热材料和环丙沙星抗菌药物，用以提高敷料的抗菌性能。因此，已有应用于伤口管理的光热敷料仍需与抗菌、促愈合药物相结合以达到伤口治疗效果，本质上无法实现非抗生素方式的光热抗菌促愈合。
基于医用敷料现状，亟需一种具有良好机械性能、光热抗菌性能、导电性能、吸水保湿性、抗氧化活性、生物相容性的综合性强的水凝胶导电敷料，为伤口提供必要的力学支撑的同时，满足伤口愈合过程中对医用敷料的非抗生素抗菌、导电促愈合的功效要求，实现对易感染伤口的治疗和管理。
发明内容
本发明解决的技术问题是：目前光热敷料仍需与抗菌、促愈合药物相结合以达到伤口治疗效果，本质上无法实现非抗生素方式的光热抗菌促愈合。
为了解决上述技术问题，本发明提供了一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料，包括棉纱布基底，所述棉纱布基底上沉积有光热组分、钙离子和导电组分，所述光热组分为聚多巴胺改性氧化石墨烯rGO@PDA，所述导电组分为聚吡咯；所述光热组分、钙离子和导电组分为交联网络结构。
本发明还提供了上述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，包括以下步骤：
步骤1：将氧化石墨烯与盐酸多巴胺加入到pH值为8.5的Tris-盐酸溶液中，在冰浴条件下进行超声分散后，混合物在磁力搅拌下反应，结束后过滤干燥得到聚多巴胺改性氧化石墨烯rGO@PDA；
步骤2：在海藻酸钠水溶液中加入交联剂、rGO@PDA并混合均匀，将棉纱布放置在该溶液中密封并静置，得到棉纱布增强水凝胶；
步骤3：将步骤2制备所得的棉纱布增强水凝胶浸于氯化铁溶液中，随后在冰浴条件下浸没于吡咯单体溶液中，使得吡咯单体原位聚合到水凝胶中，得到棉纱布增强水凝胶导电敷料rGO@PDA/SA/PPy/CG。
优选地，所述步骤1中氧化石墨烯与盐酸多巴胺的质量比为2:1，所述反应的温度为60℃，时间为24h。
优选地，所述步骤2中的海藻酸钠水溶液的浓度为0.01～0.03g/mL。
优选地，所述步骤2中的交联剂包括碳酸钙和葡萄糖内酯；其中，碳酸钙和葡萄糖内酯的质量比为0.1～1：1；所述静置的时间为24～48h。
优选地，所述步骤2中rGO@PDA和海藻酸钠的质量比为0.02～0.32：1。
优选地，所述步骤2中的棉纱布的层数为2～20层。
优选地，所述步骤3中的氯化铁溶液的浓度为0.01～1mol/L，所述吡咯单体溶液的pH值经盐酸调整到6，所述浸没的时间为12～36h。
优选地，所述步骤3中的吡咯单体与氯化铁的摩尔比为2:1。
优选地，所述步骤3中得到的棉纱布增强水凝胶导电敷料rGO@PDA/SA/PPy/CG还需经过蒸馏水清洗。
本发明与现有技术相比，具有如下有益效果：
1.本发明所制备的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料通过离子交联、物理沉积等方法，采用棉纱布增强水凝胶以提高敷料整体机械性能，为伤口提供必要的力学支撑；
2.本发明所制备的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料以聚多巴胺改性氧化石墨烯为光热组分，该光热组分光热转换率高，可以为伤口提供有效且适宜的光热作用，起到杀灭细菌的作用，预防或治疗感染性伤口，避免抗生素带来的耐药性问题；其中，聚多巴胺改性不仅有效改善了氧化石墨烯的生物相容性，并且可提供协同光热效果，保证抗菌高效性和安全性；此外，聚多巴胺也提供了一定的抗氧化活性，以清除伤口内多余的活性氧；
3.本发明所制备的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料以聚吡咯为导电组分，一方面赋予敷料良好的导电性能以促进伤口愈合，另一方面提供一定的光热抗菌效果，提高光热抗菌性能；
4.本发明所制备的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料综合性能强，同时具有良好的机械性能、有效的光热抗菌性能、导电性能、吸水保湿性、抗氧化活性和生物相容性。该敷料克服了传统棉纱布易与伤口粘连，渗出液易感染伤口等不足，同时提高了水凝胶的力学性能，能够为伤口提供了足够的力学支撑；该敷料能够维持伤口的湿润环境，为伤口愈合提供有利的微环境；该敷料同时满足伤口愈合过程中对医用敷料的非抗生素抗菌、导电促愈合的功效要求，可有效用于易感染伤口的治疗和管理。。
附图说明
图1为不同吡咯单体浓度的SA/PPy/CG的经向断裂强力/N(a)、伸长率/％(b)及纬向断裂强力/N(c)、伸长率/％(d)；
图2为不同吡咯单体浓度的SA/PPy/CG的电导率(S/m)；
图3为聚多巴胺还原氧化石墨烯过程示意图；
图5为rGO@PDA分散于棉纱布增强水凝胶网络结构示意图；
图4为GO、rGO@PDA的FTIR谱图；
图6为SA/CG、SA/PPy/CG、不同rGO@PDA:SA 质量比的rGO@PDA/SA/PPy/CG在2W/cm2的近红外光照射下的温度随时间变化曲线；
图7为SA/CG、SA/PPy/CG和不同rGO@PDA:SA质量比的rGO@PDA/SA/PPy/CG在2W/cm2的近红外光照射下对金黄色葡萄球菌S.aureus(a)和大肠杆菌E.coli(b)的光热抗菌效果。
具体实施方式
为使本发明更明显易懂，兹以优选实施例，并配合附图作详细说明如下。
实施例1
棉纱布增强导电水凝胶(SA/PPy/CG)的制备：
(1)基于CaCO3和SA(海藻酸钠)的质量比，称取一定质量的CaCO3和GDL(葡萄糖内脂)加入到SA溶液中，超声混合均匀。然后取10层5cm×5cm的棉纱布浸没其中，用保鲜膜封口静置反应24小时，得到棉纱布增强水凝胶敷料；
(2)随后，将棉纱布增强水凝胶敷料浸没于FeCl3·6H2O溶液中24小时，取出后用蒸馏水洗涤。随后敷料在冰浴条件下浸没于吡咯单体溶液中，用0.1mol/L的盐酸溶液将pH调整到6，放置6小时，蒸馏水清洗过后得到棉纱布增强水凝胶导电敷料(SA/PPy/CG)。
其中，步骤(1)中，SA溶液的浓度设为0.01g/mL、0.015g/mL、0.02g/mL、0.025g/mL，具体优选为0.02g/mL；CaCO3和SA的质量比为0.287；步骤(2)中，FeCl3·6H2O溶液浓度为0.1024mol/L。
经测试，不同吡咯单体浓度的SA/PPy/CG的经向断裂强力/N、伸长率/％、纬向断裂强力/N(c)及伸长率/％如图1所示；由图1可知，水凝胶的强力经过棉纱布的增强，在一定条件下达到了和棉纱布相近的力学性能，能够满足棉纱布增强水凝胶机械性能的要求。不同吡咯单体浓度的SA/PPy/CG的电导率(S/m)如图2所示；由图2可知，敷料获得了1.93×10-2～4.13×10-2S/m的电导率，范围符合导电水凝胶的电导率范围，并且大于人体皮肤电导率的范围(10-3～10-4S/m)，满足促进伤口愈合的电导率要求。
实施例2
一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料(rGO@PDA/SA/PPy/CG))的制备方法，包括以下步骤：
(1)将100mg的GO(氧化石墨烯)与50mg的盐酸多巴胺加入到200mL的10mM Tris-盐酸溶液中(pH＝8.5)，在冰浴条件下进行超声分散后，将混合物在60℃下磁力搅拌反应24h，结束后过滤干燥得到rGO@PDA；其中，聚多巴胺还原氧化石墨烯的过如图3所示，GO、rGO@PDA的FTIR谱图如图4所示，证明GO被盐酸多巴胺成功还原。
(2)基于CaCO3和SA的质量比为0.287，称取一定质量的CaCO3加入到12g的0.02g/mLSA溶液中，超声混合均匀。再分别称取rGO@PDA和质量分数为0.9620wt％的25g葡萄糖内酯溶液加入并混合均匀，其中，rGO@PDA与SA的质量比可设为0.02、0.04、0.08、0.16、0.32。然后取10层5cm×5cm的棉纱布浸没其中，用保鲜膜封口静置反应24小时，得到棉纱布增强水凝胶敷料；
随后，将含不同rGO@PDA的棉纱布增强水凝胶敷料分别浸没于体积为100mL、浓度为0.1024mol/L的FeCl3·6H2O溶液中24小时，取出后用蒸馏水洗涤。把浸没过铁离子的水凝胶在冰浴条件下浸没于100mL的0.0512mol/L吡咯单体溶液中，用0.1mol/L的盐酸溶液将pH调整到6，放置6小时使得吡咯单体原位聚合到水凝胶中，蒸馏水清洗过后得到棉纱布增强水凝胶导电敷料(rGO@PDA/SA/PPy/CG)，其结构如图5所示，包括棉纱布基底，棉纱布基底上沉积有光热组分聚多巴胺改性氧化石墨烯rGO@PDA、钙离子和导电组分聚吡咯，所述光热组分为，所述导电组分为；三者形成交联网络结构。
图6为SA/CG、SA/PPy/CG、不同rGO@PDA:SA质量比的rGO@PDA/SA/PPy/CG在2W/cm2的近红外光照射下的温度随时间变化曲线；经过近红外光的照射，SA/CG温度无明显变化，而SA/PPy/CG可达到40.7℃，rGO@PDA/SA/PPy/CG最高温度可达到45℃，但均低于50℃，说明了敷料具有良好的光热效果，且光热温度温和；同时证明敷料光热效果来源于rGO@PDA和PPy的协同光热效应.
图7为SA/CG、SA/PPy/CG和不同rGO@PDA:SA质量比的rGO@PDA/SA/PPy/CG在2W/cm2的近红外光照射下的金黄色葡萄球菌S.aureus(a)和大肠杆菌E.coli(b)的光热抗菌效果；rGO@PDA/SA/PPy/CG在近红外光照射下对革兰氏阴性菌和革兰氏阳性菌均具有良好光热抗菌效果；其中，当rGO@PDA与SA质量比为0.16时，近红外光照射20分钟后，金黄色葡萄球菌存活率为0.57％，大肠杆菌存活率为3.58％。
以上所述，仅为本发明的较佳实施例，并非对本发明任何形式上和实质上的限制，应当指出，对于本技术领域的普通技术人员，在不脱离本发明的前提下，还将可以做出若干改进和补充，这些改进和补充也应视为本发明的保护范围。

Claims (10)

1.一种具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料，其特征在于，包括棉纱布基底，所述棉纱布基底上沉积有光热组分、钙离子和导电组分，所述光热组分为聚多巴胺改性氧化石墨烯rGO@PDA，所述导电组分为聚吡咯；所述光热组分、钙离子和导电组分为交联网络结构。
2.权利要求1所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，包括以下步骤：
步骤1：将氧化石墨烯与盐酸多巴胺加入到pH值为8.5的Tris-盐酸溶液中，在冰浴条件下进行超声分散后，混合物在磁力搅拌下反应，结束后过滤干燥得到聚多巴胺改性氧化石墨烯rGO@PDA；
步骤2：在海藻酸钠水溶液中加入交联剂、rGO@PDA并混合均匀，将棉纱布放置在该溶液中密封并静置，得到棉纱布增强水凝胶；
步骤3：将步骤2制备所得的棉纱布增强水凝胶浸于氯化铁溶液中，随后在冰浴条件下浸没于吡咯单体溶液中，使得吡咯单体原位聚合到水凝胶中，得到棉纱布增强水凝胶导电敷料rGO@PDA/SA/PPy/CG。
3.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤1中氧化石墨烯与盐酸多巴胺的质量比为2:1，所述反应的温度为60℃，时间为24h。
4.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤2中的海藻酸钠水溶液的浓度为0.01～0.03g/mL。
5.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤2中的交联剂包括碳酸钙和葡萄糖内酯；其中，碳酸钙和葡萄糖内酯的质量比为0.1～1：1；所述静置的时间为24～48h。
6.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤2中rGO@PDA和海藻酸钠的质量比为0.02～0.32：1。
7.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤2中的棉纱布的层数为2～20层。
8.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤3中的氯化铁溶液的浓度为0.01～1mol/L，所述吡咯单体溶液的pH值经盐酸调整到6，所述浸没的时间为12～36h。
9.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述步骤3中的吡咯单体与氯化铁的摩尔比为2:1。
10.根据权利要求2所述的具有光热抗菌及促愈效果的棉纱布增强水凝胶导电敷料的制备方法，其特征在于，所述得到的棉纱布增强水凝胶导电敷料rGO@PDA/SA/PPy/CG还需经过蒸馏水清洗。
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