CN109456450A - 一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法 - Google Patents

一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法 Download PDF

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CN109456450A
CN109456450A CN201811218527.6A CN201811218527A CN109456450A CN 109456450 A CN109456450 A CN 109456450A CN 201811218527 A CN201811218527 A CN 201811218527A CN 109456450 A CN109456450 A CN 109456450A
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polycaprolactone
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但卫华
黄艳萍
但年华
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Abstract

本文公开了一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法。所述医用膜内层为聚己内酯/明胶，外层为聚己内酯和甲基丙烯酰氧乙基三甲基氯化铵原位交联后的改性聚己内酯。双层复合膜经过两步旋涂法制得。改性后的聚己内酯含有季铵基基团，赋予了其抗菌性。本发明所制备的复合膜具有良好的生物相容性和抗菌抑菌性能，在敷料、止血材料、组织工程支架材料等领域具有广泛的用途。

Description

一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医 用膜的方法
技术领域
本发明涉及一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法，属于生物医用材料制备领域。
背景技术
在伤口愈合过程中，细菌感染往往导致愈合延迟和发病率增加。因此，开发能够避免微生物生长或防止细菌渗入伤口的杀菌伤口敷料是当务之急。目前，已经生产出抗微生物药物和银纳米颗粒等多种释放型杀菌剂来抵抗感染的薄膜，微球和其他敷料物质。然而，抗菌剂的添加可能会导致机械性能的下降，由非控制释放引起的潜在的毒性，甚至增加了抗微生物药物耐药性的风险。上述缺点妨碍了释放剂的应用。
众所周知，聚季铵盐可以非常有效地抑制细菌的增殖，这归因于其有效的抗菌活性和广谱性。含有烷基链的聚季铵盐表现出优异的杀菌性能，并克服了其他抗生素制剂所显示的化学稳定性差和抗微生物药物耐药性的缺点。据报道，[2-（甲基丙烯酰氧基）乙基]三甲基氯化铵溶液（[MTA] [Cl]）具有容易进行自由基聚合，显示出突出的杀菌活性。
然而，季铵盐表现出细胞毒性的潜在风险，这可能是由于季铵基团与细胞接触时，引起的细胞膜磷脂双分子层的破坏。为了实现优异的杀菌活性和避免潜在的细胞毒性，本专利设计了双层伤口敷料。在制备双层膜的方法中，旋涂法是一种最有效和简单的方法之一。聚己内酯是一种合成的生物相容性聚合物，具有优异的机械稳定性，已被FDA生物医学应用认可，并且常用于伤口敷料，药物输送和骨修复领域。[MTA] [Cl]的抗菌部分可通过原位交联聚合接枝到聚己内酯上。原位交联聚合是使用官能单体制造功能性聚合物材料的方法。在反应过程中，功能性单体的进行聚合和交联，形成网络大分子，起到功能性的作用。原位交联聚合法比共混，涂布，接枝等膜修饰方法具有更多优点，如节省时间，避免繁琐的净化，降低原料用量，操作简便等。因此，通过原位交联聚合的方法，可以将[MTA] [Cl]引入PCL膜中以获得抗菌活性。明胶，是胶原的降解产物，来源广泛，价格低廉，具有良好的生物相容性，可促进细胞生长增殖，常用于敷料、组织工程等领域。因此，本发明使用原位聚合和旋涂法相结合的制备方法，不仅在方法上创新，而且制备的双层复合型抗菌抑菌医用膜具有良好的生物相容性和抗菌抑菌性能。
发明内容
本发明的目的是为生物医学材料领域提供一种生物相容性好、良好抗菌性的复合膜，能够应用到伤口、止血材料、组织工程支架材料等领域。
本发明的目的可以由以下制备技术来实现，其制备方法步骤如下：
（1）甲基丙烯酰氧乙基三甲基氯化铵改性聚己内酯（A）的制备：称取一定量的聚己内酯于反应釜中，溶于三氟乙醇中，配成质量浓度为5%~14%的溶液，然后将一定质量比例的偶氮二异丁腈（AIBN）、N，N′⁃亚甲基双丙烯酰胺(MBA)和甲基丙烯酰氧乙基三甲基氯化铵溶于上述聚己内酯溶液中，50~80°C下反应4~24h，即制得A液；
（2）聚己内酯/明胶共混液（B）的制备：称取一定量的聚己内酯（质量浓度为5%~14%）和明胶（质量浓度为5%~14%）于反应釜中，溶于三氟乙醇，搅拌至完全溶解，即制得B液；
（3）双层复合型抗菌抑菌医用膜的制备：吸取一定量的A液，滴于玻璃平板中心处，旋涂总时间为6~30 s，旋涂速度为60~300 rpm。在旋涂进行至3~20 s时滴加B液，旋涂至设置时间结束。将玻璃平板及平板上的覆膜置于大量蒸馏水中直至脱模；
（4）将上述双层复合型抗菌抑菌医用膜先后浸渍在生理盐水、PBS缓冲液和去离子水中，以除去残留在双层复合抗菌纤维膜中的三氟乙醇溶剂，经冷冻干燥、剂量为6~30KGy/h60Co所产生的γ射线消毒灭菌，成型包装，获得双层复合型抗菌抑菌医用膜。
在上述制备中，步骤（1）中所述的聚己内酯分子量为14000~80000 g/mol，明胶为市售分析纯及以上纯度明胶，聚己内酯与甲基丙烯酰氧乙基三甲基氯化铵的投料比为1:0~0:1， N，N′⁃亚甲基双丙烯酰胺(MBA)和甲基丙烯酰氧乙基三甲基氯化铵的投料比为1:100~1:10，偶氮二异丁腈（AIBN）和N，N′⁃亚甲基双丙烯酰胺(MBA)的投料比为1:100~1:10，聚己内酯与明胶的投料比为1:0~0:1。步骤（3）中所述的旋涂条件为：旋涂总时间为6~30 s，旋涂速度为60~300 rpm。在旋涂进行至3~20 s时滴加B液，旋涂至设置时间结束。
与现有技术相比，本发明具有以下优点：
（1）本发明采用原位交联聚合改性聚己内酯，改性方法简单省时，用料少，成本低；
（2）本发明两步旋涂法制备了双层复合型抗菌抑菌医用膜，制备方法简单，两层膜相容良好；
（3）本发明制备的双层复合型抗菌抑菌医用膜具有良好的生物相容性、抗菌活性，且便于附加抗炎、抗/肿瘤等性能，综合性能优良，功能多样，易于形成规模化产业链，取得规模化效益的良好前景。
综上所述，采用原位交联聚合改性和旋涂法制备双层复合型抗菌抑菌医用膜，本方法兼顾了使用性和生物相容性，具有明显的创新性和实用性。
具体实施方式
下面通过实施对本发明进行具体的描述，有必要在此指出的是本实施例只用于对本发明进行进一步说明，而不能理解为对发明保护范围的限制，该领域的技术熟练人员可以根据上述发明的内容作出一些非本质的改进和调整。
实施例1
（1） 甲基丙烯酰氧乙基三甲基氯化铵改性聚己内酯（A）的制备：称取一定量的聚己内酯于反应釜中，溶于三氟乙醇中，配成质量浓度为7%的溶液，然后甲基丙烯酰氧乙基三甲基氯化铵加入上述溶液中，使其质量浓度为7%，偶氮二异丁腈（AIBN）、N，N′⁃亚甲基双丙烯酰胺(MBA)的投入量分别为甲基丙烯酰氧乙基三甲基氯化铵的5%和0.1%，60°C下反应12h，即制得A液；
（2）聚己内酯/明胶共混液（B）的制备：称取一定量的聚己内酯（质量浓度为7%）和明胶（质量浓度为7%）于反应釜中，溶于三氟乙醇，搅拌至完全溶解，即制得B液；
（3）双层复合型抗菌抑菌医用膜的制备：吸取一定量的A液，滴于玻璃平板中心处，旋涂总时间为20 s，旋涂速度为100 rpm。在旋涂进行至10 s时滴加B液，旋涂至设置时间结束。将玻璃平板及平板上的覆膜置于大量蒸馏水中直至脱模；
（4）将上述双层复合型抗菌抑菌医用膜先后浸渍在生理盐水、PBS缓冲液和去离子水中，以除去残留在双层复合抗菌纤维膜中的三氟乙醇溶剂，经冷冻干燥、剂量为6~30KGy/h60Co所产生的γ射线消毒灭菌，成型包装，获得双层复合型抗菌抑菌医用膜。
实施例2
（1）甲基丙烯酰氧乙基三甲基氯化铵改性聚己内酯（A）的制备：称取一定量的聚己内酯于反应釜中，溶于三氟乙醇中，配成质量浓度为8%的溶液，然后甲基丙烯酰氧乙基三甲基氯化铵加入上述溶液中，使其质量浓度为3.5%，偶氮二异丁腈（AIBN）、N，N′⁃亚甲基双丙烯酰胺(MBA)的投入量分别为甲基丙烯酰氧乙基三甲基氯化铵的5%和0.1%，60°C下反应8h，即制得A液；
（2）聚己内酯/明胶共混液（B）的制备：称取一定量的聚己内酯（质量浓度为7%）和明胶（质量浓度为8%）于反应釜中，溶于三氟乙醇，搅拌至完全溶解，即制得B液；
（3）双层复合型抗菌抑菌医用膜的制备：吸取一定量的A液，滴于玻璃平板中心处，旋涂总时间为30 s，旋涂速度为100 rpm。在旋涂进行至8 s时滴加B液，旋涂至设置时间结束。将玻璃平板及平板上的覆膜置于大量蒸馏水中直至脱模，得到双层复合型抗菌抑菌医用膜；
（4）将上述双层复合型抗菌抑菌医用膜先后浸渍在生理盐水、PBS缓冲液和去离子水中，以除去残留在双层复合抗菌纤维膜中的三氟乙醇溶剂，经冷冻干燥、剂量为6~30KGy/h60Co所产生的γ射线消毒灭菌，成型包装，获得双层复合型抗菌抑菌医用膜。
实施例3
（1）甲基丙烯酰氧乙基三甲基氯化铵改性聚己内酯（A）的制备：称取一定量的聚己内酯于反应釜中，溶于三氟乙醇中，配成质量浓度为8%的溶液，然后甲基丙烯酰氧乙基三甲基氯化铵加入上述溶液中，使其质量浓度为4%，偶氮二异丁腈（AIBN）、N，N′⁃亚甲基双丙烯酰胺(MBA)的投入量分别为甲基丙烯酰氧乙基三甲基氯化铵的10%和0.5%，60°C下反应4h，即制得A液；
（2）聚己内酯/明胶共混液（B）的制备：称取一定量的聚己内酯（质量浓度为8%）和明胶（质量浓度为7%）于反应釜中，溶于三氟乙醇，搅拌至完全溶解，即制得B液；
（3）双层复合型抗菌抑菌医用膜的制备：吸取一定量的A液，滴于玻璃平板中心处，旋涂总时间为25 s，旋涂速度为80 rpm。在旋涂进行至10 s时滴加B液，旋涂至设置时间结束。将玻璃平板及平板上的覆膜置于大量蒸馏水中直至脱模；
（4）将上述双层复合型抗菌抑菌医用膜先后浸渍在生理盐水、PBS缓冲液和去离子水中，以除去残留在双层复合抗菌纤维膜中的三氟乙醇溶剂，经冷冻干燥、剂量为6~30KGy/h60Co所产生的γ射线消毒灭菌，成型包装，获得双层复合型抗菌抑菌医用膜。

Claims (3)

1.一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法，特征在于，其制备方法包括如下步骤：
甲基丙烯酰氧乙基三甲基氯化铵改性聚己内酯（A）的制备：称取一定量的聚己内酯于反应釜中，溶于三氟乙醇中，配成质量浓度为5%~14%的溶液，然后将一定质量比例的偶氮二异丁腈（AIBN）、N，N′⁃亚甲基双丙烯酰胺(MBA)和甲基丙烯酰氧乙基三甲基氯化铵溶于上述聚己内酯溶液中，50~80°C下反应4~24h，即制得A液；
聚己内酯/明胶共混液（B）的制备：称取一定量的聚己内酯（质量浓度为5%~14%）和明胶（质量浓度为5%~14%）于反应釜中，溶于三氟乙醇，搅拌至完全溶解，即制得B液；
双层复合型抗菌抑菌医用膜的制备：吸取一定量的A液，滴于玻璃平板中心处，旋涂总时间为6~30 s，旋涂速度为60~300 rpm；在旋涂进行至3~20 s时滴加B液，旋涂至设置时间结束；将玻璃平板及平板上的覆膜置于大量蒸馏水中直至脱模；
将上述双层复合型抗菌抑菌医用膜先后浸渍在生理盐水、PBS缓冲液和去离子水中，以除去残留在双层复合型抗菌医用膜中的三氟乙醇溶剂，经冷冻干燥、剂量为6~30KGy/h60Co所产生的γ射线消毒灭菌，成型包装，获得双层复合型抗菌抑菌医用膜。
2.权利要求1所述一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法，其特征在于，步骤（1）中所述的聚己内酯分子量为14000~80000 g/mol，明胶为市售分析纯及以上纯度明胶；
聚己内酯与甲基丙烯酰氧乙基三甲基氯化铵的投料比为1:0~0:1，N,N′⁃亚甲基双丙烯酰胺(MBA)和甲基丙烯酰氧乙基三甲基氯化铵的投料比为1:100~1:10，偶氮二异丁腈（AIBN）和N，N′⁃亚甲基双丙烯酰胺(MBA)的投料比为1:100~1:10，聚己内酯与明胶的投料比为1:0~0:1。
3.根据权利要求1所述一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法，其特征在于，步骤（3）中所述的旋涂条件为：旋涂总时间为6~30 s，旋涂速度为60~300 rpm；在旋涂进行至3~20 s时滴加B液，旋涂至设置时间结束。
CN201811218527.6A 2018-10-19 2018-10-19 一种基于旋涂法和原位交联聚合制备双层复合型抗菌抑菌医用膜的方法 Pending CN109456450A (zh)

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