CN113563643A - 缓释抗菌的交联壳聚糖/蒙脱石薄膜及其制备方法 - Google Patents
缓释抗菌的交联壳聚糖/蒙脱石薄膜及其制备方法 Download PDFInfo
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- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 44
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Abstract
本发明公开了一种缓释抗菌的交联壳聚糖/蒙脱石薄膜及其制备方法，包括：将抗菌剂溶解于醇溶剂中，再加入蒙脱石，混匀后去除醇溶剂，得到蒙脱石负载型抗菌剂；将交联剂缓慢滴加到醋酸溶解的壳聚糖溶液中混匀后再加入甘油得混合液；将蒙脱石负载型抗菌剂加入混合液中混匀，得到成膜液；之后平铺干燥成膜。本发明交联壳聚糖/蒙脱石薄膜是以交联壳聚糖、蒙脱石形成膜的基本结构，以甘油作为增塑剂，增加膜的柔韧性，最后平铺干燥，揭膜即得缓释抗菌的交联壳聚糖/蒙脱石薄膜。本发明的交联壳聚糖/蒙脱石薄膜具有缓释性，PH响应性，透气性能好，可根据不同需求调节缓释膜的缓释速率，满足不同的需求。
Description
技术领域
本发明属于生物医用材料领域，具体涉及一种具有缓释抗菌性能的交联壳聚糖/蒙脱石薄膜及其制备方法。
背景技术
生物医用材料中的伤口敷料和组织工程材料，每年可创造巨大经济价值。伤口敷料因其具有促进伤口愈合、防止细菌感染、透气保湿等优点而受到广泛关注。其中，抗菌活性是一项重要的性能指标，要求敷料具有持久的抗菌、抗炎作用。同时，应控制药物释放速率，以确保长期疗效。因此，优良的抗菌活性和持久的释放性能对伤口敷料尤为重要。抗菌剂缓释薄膜可有效控制活性成分的释放，延长抗菌剂的药效期，降低抗菌剂用量。水蒸气透过率是伤口敷料质量的一个重要指标。研究表明，每天2000–2500g/m2的水蒸气透过率可提供足够的水分，防止伤口脱水。较高的水蒸气透过率会使伤口迅速干燥并产生疤痕，而较低的水蒸气透过率导致伤口分泌物积聚，伤口愈合速度减慢，伤口感染风险增加。
壳聚糖是甲壳素的N-脱乙酰化形式，具有良好的亲水性、生物相容性、可生物降解性和吸附性，还具有良好的抗菌性能，但壳聚糖单独成膜柔韧性差，机械强度差，易溶解，因此很难制成薄膜使用。戊二醛是一种化学交联剂，将戊二醛添加到壳聚糖溶液中，戊二醛与壳聚糖大分子链上的亲水性基团氨基和羟基反应，形成交联结构，交联后的产物不易溶胀，以此来调节壳聚糖膜的溶胀性能，改善膜的疏水性能。目前膜的研究主要是在塑料、食品方面，尚缺乏在医学应用方面的研究。
发明内容
本发明针对现有技术的不足，提供了一种具有缓释抗菌性能的交联壳聚糖/蒙脱石薄膜及其制备方法，本发明的原材料资源丰富，价格低廉，可根据需求调节载药薄膜释放速率，满足不同的需求，具有较好的发展前景。
为实现上述目的，本发明采用如下的技术方案：
一种缓释抗菌的交联壳聚糖/蒙脱石薄膜的制备方法，包括如下步骤：
(1)将抗菌剂溶解于醇溶剂中，再加入蒙脱石，混合均匀后去除所述醇溶剂，得到蒙脱石负载型抗菌剂；
(2)将交联剂缓慢滴加到醋酸溶解的壳聚糖溶液中混匀后再加入甘油得混合液；
(3)将所述蒙脱石负载型抗菌剂加入所述混合液中混匀，得到成膜液；
(4)将所述成膜液平铺在模具上，干燥后即得。
优选的，所述制备方法中，各原料的质量用量为：
壳聚糖1～6份，交联剂0.005～0.02份，甘油0.1～0.5份，醋酸1～5份，蒙脱石0.01～0.05份，抗菌剂0.01～0.3份。
优选的，所述抗菌剂为醋酸氯己定。
优选的，所述醋酸的浓度为1～5wt％，更优选为2～4wt％。
优选的，所述交联剂为戊二醛。
优选的，步骤(1)中去除醇溶剂的方法为挥干。
优选的，步骤(1)所述醇溶剂为乙醇、甲醇中的一种或两种。
优选的，步骤(1)中所述混合均匀的方法为搅拌，优选的，所述搅拌的时间为12h～48h。
优选的，步骤(1)还包括去除醇溶剂后真空干燥的步骤，优选的，所述真空干燥为在40～60℃条件下真空干燥8～24h。
优选的，步骤(2)中所述混匀的方法为以50～300rpm的速度搅拌0.5～2h。
优选的，步骤(3)还包括加入所述蒙脱石负载型抗菌剂后搅拌6h～24h的步骤。
优选的，步骤(4)中所述模具为干燥、洁净的模具。
优选的，步骤(4)中所述成膜液平铺在模具上，形成厚薄均匀、表面光洁平整的液层。
优选的，步骤(4)所述的干燥为在40～70℃的烘箱中干燥6h～24h。
本发明还提供上述制备方法制备得到的交联壳聚糖/蒙脱石薄膜。
本发明的交联壳聚糖/蒙脱石薄膜中，蒙脱石是一种纳米厚度的表面带负电的硅酸盐片层，具有独特的层状结构和阳离子交换特性，从而赋予其一定的吸附能力，作为抗菌剂的载体而存在；甘油作为增塑剂，赋予膜一定的韧性。交联剂与壳聚糖发生交联，调节壳聚糖膜的溶胀性能。蒙脱石吸附抗菌剂，使药物缓慢释放，达到持久释放的目的。这些组分的组合以及各组分的上述混合范围，通过大量实验确定。
本发明通过浸入PBS缓冲液法测量载药膜的药物缓释性能。
与现有技术相比，本发明具有如下有益效果：
本发明用抗菌剂(醋酸氯己定)吸附在蒙脱石表面，起到延缓药物释放的作用。蒙脱石具有独特的层状结构，优良的吸附性能，能有效抑制药物分子的扩散，使得壳聚糖/蒙脱石缓释薄膜的缓释性能大幅度提高。
1.本发明的壳聚糖/蒙脱石缓释薄膜可根据蒙脱石的含量、使用环境的PH值来调节薄膜的释放速率，因而能满足不同的需要。
2.本发明的壳聚糖/蒙脱石缓释薄膜具有缓释性、PH响应性，可作为一种具有广阔前景的抗菌伤口敷料。
3.本发明的壳聚糖/蒙脱石缓释薄膜中的抗菌剂可缓慢地释放，发挥药效，蒙脱石可有效降低其释放速率，延长其药效期。
4.本发明的薄膜水蒸气透过率在每天2000g/m2以上，无需使用传统凝胶的基底，且透气性比其更好。
附图说明
图1是实施例1中制得的缓释薄膜和不含蒙脱石的薄膜在PH为7.4的PBS缓冲液中醋酸氯己定的累积释放曲线图。
图2是实施例1中制得的缓释薄膜分别在PH为7.4和8.0的PBS缓冲液中醋酸氯己定的累积释放度曲线。
图3是实施例2中制得的缓释薄膜在PH为7.4的PBS缓冲液中醋酸氯己定的累积释放度曲线。具体实施方式
以下结合实例对本发明的具体实施作进一步的说明，但本发明的实施方式不限于此。
实施例1
将0.02g醋酸氯己定溶解于甲醇中，再加入0.01g蒙脱石，搅拌24h，挥干有机溶剂，将产物50℃条件下真空干燥24h，得蒙脱石负载的醋酸氯己定，备用。
在250mL烧杯中，加入1g壳聚糖、100mL2wt％的醋酸溶液，搅拌6h，形成溶液，此后将2mL0.25wt％戊二醛水溶液缓慢滴加到上述溶液中，在室温下以150rpm的速度温和搅拌1h，然后加入0.1g甘油，以350rpm的转速搅拌2h，此后将上述制备的蒙脱石负载的醋酸氯己定加入到混合溶液中，继续搅拌12h，得成膜液。
将制得的成膜液均匀地平铺在干燥、洁净的模具上，形成厚薄均匀，表面光洁平整的液层，在50℃的烘箱中干燥，干燥时间为12h，揭膜即得具有缓释性能的交联壳聚糖/蒙脱石薄膜。
图1是实施例1中制得的缓释薄膜和不含蒙脱石的薄膜在PH为7.4的PBS缓冲液中醋酸氯己定的累积释放度曲线。从图1可看出，蒙脱石负载醋酸氯己定，可明显降低其释放速率，延长其释放时间，提高其缓释性能。在前期阶段(0-1h)，醋酸氯己定从缓释膜中的释放速率较快，当浸入PH为7.4的PBS缓冲液1h时，累积释放度为20.1％，而此时不采用蒙脱石负载的醋酸氯己定缓释膜中醋酸氯己定的累积释放度达41.5％。随后醋酸氯己定的释放速率逐渐降低，当浸入时间为8h，累积释放百分比为28.1％。
图2是实施例1中制得的缓释薄膜分别在PH为7.4和8.0的PBS缓冲液中醋酸氯己定的累积释放度曲线。从图2可看出，缓释薄膜浸入PH为7.4的PBS缓冲液8h，醋酸氯己定的累积释放度为28.1％，当浸入PH为8.0的PBS缓冲液8h时，醋酸氯己定的累积释放度为20.0％，缓释薄膜具有一定的PH响应性。
将薄膜样品剪切成大小合适的形状，将其放在装有20g无水氯化钙的量杯顶部并用封口膜将边缘封紧，计算得到薄膜样品的面积S(4.52×10-4m2)，称取此时量杯的质量。然后将密封好的量杯放入到装有200ml蒸馏水的密封容器中，密封容器置于40℃烘箱中，24h后取出量杯再次称其质量，计算得到量杯质量变化ΔM(1.10g)，利用公式：水蒸气透过率(WVTR)＝ΔM/S，测得薄膜水蒸气透过率为每天2434g/m2。
实施例2
将0.3g醋酸氯己定溶解于甲醇中，再加入0.03g蒙脱石，搅拌48h，挥干有机溶剂，将产物40℃条件下真空干燥16h，得蒙脱石负载的醋酸氯己定，备用。
在250mL烧杯中，加入6g壳聚糖、100mL5wt％的醋酸溶液，搅拌8h，形成溶液，此后将2mL1wt％戊二醛水溶液缓慢滴加到上述溶液中，在室温下以300rpm的速度温和搅拌0.5h，然后加入0.5g甘油，以350rpm的转速搅拌2h，此后将上述制备的蒙脱石负载的醋酸氯己定加入到混合溶液中，继续搅拌6h，得成膜液。
图3是实施例2中制得的缓释薄膜在PH为7.4的PBS缓冲液中醋酸氯己定的累积释放度曲线。从图3可看出，在前期(0-3h)，醋酸氯己定从缓释膜中的释放速率较快，当浸入PH为7.4的PBS缓冲液3h时，累积释放度为19.4％，当浸入时间为8h，累积释放度为22.6％。将薄膜样品剪切成大小合适的形状，将其放在装有20g无水氯化钙的量杯顶部并用封口膜将边缘封紧，计算得到薄膜样品的面积S(4.52×10-4m2)，称取此时量杯的质量。然后将密封好的量杯放入到装有200ml蒸馏水的密封容器中，密封容器置于40°烘箱中，24h后取出量杯再次称其质量，计算得到量杯质量变化ΔM(0.99g)，利用式子水蒸气透过率(WVTR)＝ΔM/S,测得薄膜水蒸气透过率为每天2190g/m2。
实施例3
将0.01g醋酸氯己定溶解于甲醇中，再加入0.05g蒙脱石，搅拌12h，挥干有机溶剂，将产物60℃条件下真空干燥8h，得蒙脱石负载的醋酸氯己定，备用。
在250mL烧杯中，加入1g壳聚糖、100mL1wt％的醋酸溶液，搅拌6h，形成溶液，此后将2mL0.5wt％戊二醛水溶液缓慢滴加到上述溶液中，在室温下以50rpm的速度温和搅拌2h，然后加入0.2g甘油，以400rpm的转速搅拌2h，此后将上述制备的蒙脱石负载的醋酸氯己定加入到混合溶液中，继续搅拌24h，得成膜液。
将制得的成膜液均匀地平铺在干燥、洁净的模具上，形成厚薄均匀，表面光洁平整的液层，在70℃的烘箱中干燥，干燥时间为6h，揭膜即得具有缓释性能的交联壳聚糖/蒙脱石薄膜。采用浸入PH为7.4的PBS缓冲液测得缓释薄膜中醋酸氯己定的累积释放曲线，实验表明，在前期(0-3h)，醋酸氯己定从缓释膜中的释放速率较快，当浸入PH为7.4的PBS缓冲液3h时，累积释放百分比为14.8％，当浸入时间为8h，累积释放百分比为18.3％。
将薄膜样品剪切成大小合适的形状，将其放在装有20g无水氯化钙的量杯顶部并用封口膜将边缘封紧，计算得到薄膜样品的面积S(4.52×10-4m2)，称取此时量杯的质量。然后将密封好的量杯放入到装有200ml蒸馏水的密封容器中，密封容器置于40°烘箱中，24h后取出量杯再次称其质量，计算得到量杯质量变化ΔM(0.91g)，利用式子水蒸气透过率(WVTR)＝ΔM/S,测得薄膜水蒸气透过率为每天2013g/m2。
Claims (10)
1.一种缓释抗菌的交联壳聚糖/蒙脱石薄膜的制备方法，包括如下步骤：
（1）将抗菌剂溶解于醇溶剂中，再加入蒙脱石，混合均匀后去除所述醇溶剂，得到蒙脱石负载型抗菌剂；
（2）将交联剂缓慢滴加到醋酸溶解的壳聚糖溶液中混匀后再加入甘油得混合液；
（3）将所述蒙脱石负载型抗菌剂加入所述混合液中混匀，得到成膜液；
（4）将所述成膜液平铺在模具上，干燥后即得。
2.根据权利要求1所述的制备方法，其特征在于，各原料的质量用量为：
壳聚糖1~6份，交联剂0.005~0.02份，甘油0.1~0.5份，醋酸1~5份，蒙脱石0.01~0.05份，抗菌剂0.01~0.3份。
3.根据权利要求1所述的制备方法，其特征在于，所述抗菌剂为醋酸氯己定。
4.根据权利要求1所述的制备方法，其特征在于，所述醋酸的浓度为0~5wt%，更优选为2~4wt%。
5.根据权利要求1所述的制备方法，其特征在于，所述交联剂为戊二醛。
6.根据权利要求1所述的制备方法，其特征在于，步骤（1）所述醇溶剂为乙醇或甲醇中的一种或两种。
7.根据权利要求1所述的制备方法，其特征在于，步骤（1）还包括去除醇溶剂后真空干燥的步骤，优选的所述真空干燥为在40~60℃条件下真空干燥8~24h。
8.根据权利要求1所述的制备方法，其特征在于，步骤（2）中所述混匀的方法为以50~300rpm的速度搅拌0.5~2h。
9.根据权利要求1所述的制备方法，其特征在于，步骤（4）所述的干燥为在40~70℃的烘箱中干燥6h~24h。
10.权利要求1-9任一所述的制备方法制备得到的交联壳聚糖/蒙脱石薄膜。
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| CN106867164A (zh) * | 2017-01-20 | 2017-06-20 | 华南理工大学 | 一种具有除草剂控释性能的pva/淀粉缓释薄膜及其制备方法 |
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| CN106867164A (zh) * | 2017-01-20 | 2017-06-20 | 华南理工大学 | 一种具有除草剂控释性能的pva/淀粉缓释薄膜及其制备方法 |
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