CN112724459B - 一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法 - Google Patents

一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法 Download PDF

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CN112724459B
CN112724459B CN202011589791.8A CN202011589791A CN112724459B CN 112724459 B CN112724459 B CN 112724459B CN 202011589791 A CN202011589791 A CN 202011589791A CN 112724459 B CN112724459 B CN 112724459B
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王铁刚
左桂福
王丹丹
刘文财
王红霞
李�浩
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Tangshan Boshide Medical Devices Co ltd
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Abstract

本发明提供了一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，包括以下步骤：(1)制备高分子水溶液；(2)抗菌液体的制备；(3)抗菌海绵的制备；(4)配置水凝胶溶液；(5)抗菌水凝胶的制备。该方法可以实现抗菌剂的均匀分散，同时可以通过水溶性高分子材料的成分和比例调控实现抗菌成分的可控释放。本发明制备形成的复合型水凝胶具有较好的抗菌稳定性和抗菌持久性，同时多孔海绵可以实现更高的锁水和力学增强作用。

Description

一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法
技术领域
本发明涉及生物医用材料领域，尤其涉及一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法。
背景技术
医用水凝胶半通透性，具有阻隔细菌，防止创面感染，允许氧气和水通过等效果。
实践证实，水凝胶对于创伤伤口的恢复具有比常规敷料更好的促进作用，但是水凝胶中的水分容易滋生细菌，创口处的血液和组织液也会滋生细菌繁殖，容易造成感染。因此，为了抑制细菌滋生，减少伤口感染几率，开发具有抗菌功能的水凝胶尤为重要。
目前常规的抗菌水凝胶技术主要分为本征型抗菌水凝胶和添加型抗菌水凝胶。其中本征型抗菌水凝胶多为具有抗菌性能的高分子材料如壳聚糖，这种技术抗菌效率有限。添加型抗菌水凝胶是采用共混方法将抗菌剂加入到水凝胶基体中，这种技术容易造成抗菌剂分散不均匀和释放不可控，影响抗菌水凝胶的抗菌效率和使用周期。
本发明采用两步法制备抗菌剂均匀分散且释放可控的抗菌水凝胶。
发明内容
有鉴于此，本发明提供了一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法。该方法可以实现抗菌剂的均匀分散，同时可以通过水溶性高分子材料的成分和比例调控实现抗菌成分的可控释放。
本发明提供的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，包括以下步骤：
(1)制备高分子水溶液：将水溶性高分子溶于去离子水中，配制成质量浓度为0.5wt％-5wt％的高分子水溶液；
(2)抗菌液体的制备：称取步骤(1)所述的高分子水溶液，并加入抗菌剂，然后常温搅拌0.5-2h，搅拌速度100-800r/min，制得抗菌液体；
(3)抗菌海绵的制备：将步骤(2)制备的抗菌液体在0℃以下冷冻0.5-5h，冻成冰水混合物的状态；然后在冷冻干燥机中进行冷冻干燥30-40h，制备抗菌海绵；
(4)配置水凝胶溶液：称取步骤(1)所述的水溶性高分子溶液，并加入0.1wt％-1wt％的交联剂，得到水凝胶溶液；
(5)抗菌水凝胶的制备：将步骤(3)所述的抗菌海绵浸渍在步骤(4)所述的水凝胶溶液中，并采用真空除泡方式去除气泡，室温下保持0.5-3h，完成水凝胶交联固化，即制得本发明的抗菌水凝胶。
优选的，步骤(1)中所述水溶性高分子材料为羧甲基纤维素钠、聚乙烯醇、羧甲基壳聚糖、海藻酸钠、明胶中的一种或多种。
优选的，步骤(2)中所述抗菌剂为纳米氧化锌、纳米氧化钛、纳米银、二氧化氯前驱体中的任意一种。
优选的，步骤(2)中抗菌剂与高分子材料的质量比例为0.1:10～3:10。
优选的，步骤(3)冷冻干燥机中的冷冻条件为温度-50℃，真空度20Pa。
优选的，步骤(4)中所述交联剂为氯化钙、戊二醛、京尼平、硼砂中的任意一种。
本发明提供的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，采用两步法制备抗菌剂均匀分散且释放可控的抗菌水凝胶。首先，将抗菌剂加入到水溶性高分子溶液中，通过冷冻干燥或其他造孔技术制备高分子抗菌多孔海绵。其次，用配置好的水凝胶液体浸渍抗菌海绵，形成抗菌水凝胶。
本发明与现有技术相比，具有以下有益效果：
本发明提供的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，可以实现抗菌剂的均匀分散，同时可以通过水溶性高分子材料的成分和比例调控实现抗菌成分的可控释放。制备形成的复合型水凝胶具有较好的抗菌稳定性和抗菌持久性，同时多孔海绵可以实现更高的锁水和力学增强作用。
附图说明
图1表示抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法示意图。
具体实施方式
以下结合实施例对本发明提供的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法进行进一步说明。
实施例1
一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，包括以下步骤：
(1)制备高分子水溶液：将水溶性高分子羧甲基纤维素钠溶于去离子水中，配制成质量浓度为2wt％的高分子水溶液；
(2)抗菌液体的制备：称取步骤(1)中的高分子水溶液100mL，并加入抗菌剂纳米氧化锌10g，然后常温搅拌1h，搅拌速度500r/min，制得抗菌液体；
(3)抗菌海绵的制备：将步骤(2)制备的抗菌液体在0℃以下冷冻3h，冻成冰水混合物的状态；然后在-50℃，真空度20Pa的条件下，于冷冻干燥机中进行冷冻干燥30h，制备抗菌海绵；
(4)配置水凝胶溶液：称取步骤(1)制备的水溶性高分子溶液，并加入0.5wt％的交联剂戊二醛，得到水凝胶溶液；
(5)抗菌水凝胶的制备：将步骤(3)制备的抗菌海绵浸渍在步骤(4)制备的水凝胶溶液中，并采用真空除泡方式去除气泡，室温下保持2h，完成水凝胶交联固化，即制得本发明的抗菌水凝胶。
实施例2
(1)制备高分子水溶液：将海藻酸钠溶于去离子水中，配制成质量浓度为1wt％的高分子水溶液；
(2)抗菌液体的制备：称取步骤(1)中的高分子水溶液100mL，并加入抗菌剂二氧化氯前驱体亚氯酸钠5g，然后常温搅拌1h，搅拌速度800r/min，制得抗菌液体；
(3)抗菌海绵的制备：将步骤(2)制备的抗菌液体在0℃以下冷冻3h，冻成冰水混合物的状态；然后在-50℃，真空度20Pa的条件下，于冷冻干燥机中进行冷冻干燥30h，制备抗菌海绵；
(4)配置水凝胶溶液：称取步骤(1)制备的水溶性高分子溶液，并加入1wt％的交联剂氯化钙，得到水凝胶溶液；
(5)抗菌水凝胶的制备：将步骤(3)制备的抗菌海绵浸渍在步骤(4)制备的水凝胶溶液中，并采用真空除泡方式去除气泡，室温下保持2h，完成水凝胶交联固化，即制得本发明的抗菌水凝胶。
实施例3
(1)制备高分子水溶液：将壳聚糖溶于去离子水中，配制成质量浓度为5wt％的高分子水溶液；
(2)抗菌液体的制备：称取步骤(1)中的高分子水溶液100mL，并加入抗菌剂纳米银0.1g，然后常温搅拌1h，搅拌速度500r/min，制得抗菌液体；
(3)抗菌海绵的制备：将步骤(2)制备的抗菌液体在0℃以下冷冻3h，冻成冰水混合物的状态；然后在-50℃，真空度20Pa的条件下，于冷冻干燥机中进行冷冻干燥30h，制备抗菌海绵；
(4)配置水凝胶溶液：称取步骤(1)制备的水溶性高分子溶液，并加入0.5wt％的交联剂戊二醛，得到水凝胶溶液；
(5)抗菌水凝胶的制备：将步骤(3)制备的抗菌海绵浸渍在步骤(4)制备的水凝胶溶液中，并采用真空除泡方式去除气泡，室温下保持2h，完成水凝胶交联固化，即制得本发明的抗菌水凝胶。
实施例4
(1)制备高分子水溶液：将聚乙烯醇溶于去离子水中，配制成质量浓度为2wt％的高分子水溶液；
(2)抗菌液体的制备：称取步骤(1)中的高分子水溶液100mL，并加入抗菌剂纳米氧化钛30g，然后常温搅拌1h，搅拌速度500r/min，制得抗菌液体；
(3)抗菌海绵的制备：将步骤(2)制备的抗菌液体在0℃以下冷冻3h，冻成冰水混合物的状态；然后在-50℃，真空度20Pa的条件下，于冷冻干燥机中进行冷冻干燥30h，制备抗菌海绵；
(4)配置水凝胶溶液：称取步骤(1)制备的水溶性高分子溶液，并加入0.5wt％的交联剂戊二醛，得到水凝胶溶液；
(5)抗菌水凝胶的制备：将步骤(3)制备的抗菌海绵浸渍在步骤(4)制备的水凝胶溶液中，并采用真空除泡方式去除气泡，室温下保持2h，完成水凝胶交联固化，即制得本发明的抗菌水凝胶。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (4)

1.一种抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，其特征在于，包括以下步骤：
（1）制备高分子水溶液：将水溶性高分子材料溶于去离子水中，配制成质量浓度为0.5wt%-5wt%的高分子水溶液；
（2）抗菌液体的制备：称取步骤（1）所述的高分子水溶液，并加入抗菌剂，然后常温搅拌0.5-2h，搅拌速度100-800r/min，制得抗菌液体；
（3）抗菌海绵的制备：将步骤（2）制备的抗菌液体在0℃以下冷冻0.5-5h，冻成冰水混合物的状态；然后在冷冻干燥机中进行冷冻干燥30-40h，制备抗菌海绵；
（4）配置水凝胶溶液：称取步骤(1)所述的高分子水溶液，并加入0.1wt%-1wt%的交联剂，得到水凝胶溶液；
（5）抗菌水凝胶的制备：将步骤（3）所述的抗菌海绵浸渍在步骤（4）所述的水凝胶溶液中，并采用真空除泡方式去除气泡，室温下保持0.5-3h，完成水凝胶交联固化，即制得抗菌水凝胶；
步骤（2）中抗菌剂与水溶性高分子材料的质量比例为0.1:10~3:10；
步骤（3）冷冻干燥机中的冷冻条件为温度-50℃，真空度20Pa。
2.根据权利要求1所述的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，其特征在于，步骤（1）中所述水溶性高分子材料为羧甲基纤维素钠、聚乙烯醇、羧甲基壳聚糖、海藻酸钠、明胶中的一种或多种。
3.根据权利要求1所述的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，其特征在于，步骤（2）中所述抗菌剂为纳米氧化锌、纳米氧化钛、纳米银、二氧化氯前驱体中的任意一种。
4.根据权利要求1所述的抗菌剂均匀分散且释放可控的抗菌水凝胶的制备方法，其特征在于，步骤（4）中所述交联剂为氯化钙、戊二醛、京尼平、硼砂中的任意一种。
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