CN112353754B - 一种导电聚吡咯/中药复合水凝胶及其制备方法与应用 - Google Patents
一种导电聚吡咯/中药复合水凝胶及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种导电聚吡咯/中药复合水凝胶及其制备方法与应用。所述方法为:以聚吡咯水凝胶为主体结构,将中药分子作为掺杂剂掺杂进水凝胶网络中,制得具有促伤口愈合功能的抑菌止血皮肤敷料。本发明制备方法简单,成本较低,且反应条件易控;所得复合水凝胶生物相容性好,有一定的抗菌效果和促细胞增殖、黏附效果,是一种很好的皮肤敷料材料。
Description
技术领域
本发明属于医用生物材料的技术领域,具体涉及一种导电聚吡咯/中药复合水凝胶及其制备方法与应用。
背景技术
皮肤是人体的一道屏障,其作用是保护人体、排出废物、调节体温等。皮肤直接与外部环境接触,很容易受到外部损伤(如大面积烧伤、创伤以及手术创口),从而造成皮肤溃烂、溃疡、出血以及过敏反应。通常这些创面需要很长的时间才能愈合,而敷料的作用在于将创面暂时与外界环境隔绝开,给皮肤修复提供一个相对独立的环境,避免二次刺激,促进伤口修复。
传统敷料大多用医用纱布,廉价易得,但容易与皮肤渗出物粘连,换药时容易对皮肤造成二次伤害。此外,医用纱布无法实现药物的长期作用,需要多次换药。水凝胶材料由于其优异的生物相容性和浸润性被广泛应用在生物医学领域。单一水凝胶敷料具有一定的透气性和浸润性,生物相容性好,不与创面造成粘连,此外可以实现药物缓释,但单一水凝胶敷料对细菌无抑制作用,容易细菌感染并产生炎症反应。所以目前研究最多的是抗菌性复合水凝胶。已有研究使用银、铜等金属纳米粒子修饰水凝胶以获得抗菌性,但原料成本较高;还有研究者基于氨基酸、二硫二吡啶和铝盐三种原料获得了抗菌率良好的水凝胶敷料,但制作过程较为复杂,且功能单一。此外这些敷料均没有促进细胞增殖黏附以促进伤口愈合的功能,限制了水凝胶敷料的应用。
发明内容
为解决现有技术的缺点和不足之处,本发明的首要目的在于提供一种导电聚吡咯/中药复合水凝胶的制备方法。本发明以聚吡咯水凝胶为主体结构,将中药分子作为掺杂剂掺杂进水凝胶网络中,赋予导电聚吡咯水凝胶抗菌、止血等功能。
本发明的另一目的在于提供由上述方法得到的一种导电聚吡咯/中药复合水凝胶。
本发明的再一目的在于提供上述一种导电聚吡咯/中药复合水凝胶在药物制备中的应用。
本发明目的通过以下技术方案实现:
一种导电聚吡咯/中药复合水凝胶的制备方法,包括以下步骤:
(1)将吡咯单体溶于极性有机溶剂中,再加入中药粉末,得到吡咯混合溶液;
(2)0~8℃下,将吡咯混合溶液与氧化剂水溶液在模板中迅速混合,搅拌一段时间后,静置,得到含杂质的聚吡咯水凝胶膜,洗涤,干燥,得到导电聚吡咯/中药复合水凝胶。
优选地,步骤(1)所述极性有机溶剂为异丙醇。
优选地,步骤(1)所述吡咯单体和中药的比例为85μL:10~150mg;所述吡咯单体和氧化剂的摩尔比为2:1~1:3。
优选地,步骤(1)所述吡咯单体在异丙醇中的浓度为0.5~3mol/L。
优选地,步骤(1)所述中药粉末为黄芩苷、黄连素、姜黄素和人参皂苷中的至少一种。
优选地,步骤(2)所述氧化剂水溶液的浓度为0.5~3mol/L。
优选地,步骤(2)所述氧化剂水溶液中的氧化剂为过硫酸铵和氧化铁中的至少一种。
优选地,步骤(2)所述搅拌的时间为2~10秒,所述静置的时间为1~10分钟。
优选地,步骤(2)所述洗涤指将含杂质的聚吡咯水凝胶膜依次在乙醇和水中浸泡,以去除多余的掺杂剂(中药粉末)和副产物。
优选地,步骤(2)所述干燥指在30~120℃下真空干燥或者冷冻干燥,此处的真空条件和冷冻干燥的条件为常规条件。
上述方法制得的一种导电聚吡咯/中药复合水凝胶。
上述一种导电聚吡咯/中药复合水凝胶在药物制备中的应用。
本发明构建了一种中药分子掺杂的导电复合水凝胶,用作止血抗菌复合水凝胶敷料,同时还能促进伤口愈合。聚吡咯是一种导电聚合物,具有很高的电导率和良好的生物相容性,能够促进细胞黏附增殖。中药分子(如黄芩苷、黄连素、姜黄素等)具有抑菌、抗炎、止血等作用,将其作为掺杂剂与聚吡咯合成促伤口愈合的抗菌复合水凝胶,开发出中药分子的新应用途径,解决了现有伤口敷料的缺陷和不足。
与现有技术相比,本发明具有以下优点及有益效果:
(1)本发明采用导电聚吡咯水凝胶为主体材料,具有优异的电化学活性,促进细胞增殖、黏附,从而促进伤口修复,加快皮肤愈合的速度,水凝胶结构具有一定的孔隙率,允许药物分子缓慢释放,延长药物作用时间,减少换药次数。
(2)中药分子具有抑菌止血的作用,使敷料在保护伤口的同时能起到消炎抑菌止血的功能。
(3)本发明的方法简单,成本较低,可以大量制备,且功能全面,克服了现有技术的缺陷与不足,实现了一种可同时满足促伤口愈合、抑菌止血的多功能皮肤敷料。
附图说明
图1为本发明所述导电聚吡咯/中药复合水凝胶的制备方法流程图。
图2为实施例1制备的导电聚吡咯/中药复合水凝胶的实物图。
图3为实施例1制备的导电聚吡咯/中药复合水凝胶的SEM图。
图4为实施例2得到的导电聚吡咯/中药复合水凝胶对大肠杆菌的作用效果图。
图5为对比例1~3制备的导电聚吡咯/中药复合水凝胶的实物图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
本发明实施例中未注明具体条件者,按照常规条件或者制造商建议的条件进行。所用未注明生产厂商者的原料、试剂等,均为可以通过市售购买获得的常规产品。
实施例1
一种导电聚吡咯/中药复合水凝胶的制备方法,包括以下步骤:
(1)取冰块放置于泡沫箱中,以维持低温环境。
(2)溶液A的准备:移取85μL的吡咯单体加入到1ml的异丙醇中,磁力搅拌使其混合均匀;再称取0.03g中药(分别为黄芩苷、黄连素、姜黄素和人参皂苷)粉末溶于上述溶液,在室温下磁力搅拌,待溶解完全后放入上述泡沫箱中,低温保存以待使用。
(3)溶液B的准备:称取0.274g过硫酸铵粉末加入到2ml去离子水中,在室温下磁力搅拌,待溶解完全后放入上述泡沫箱中,低温保存以待使用。
(4)用移液枪先后取70μL溶液A和140μL溶液B,加入到圆形模板中,搅拌10秒,静置1分钟,此时溶液凝固成胶状结构,得到含有杂质的聚吡咯水凝胶膜。为了除去多余的掺杂剂和副产物,将产物依次放入乙醇和去离子水中纯化12h和24h,取出产物冷冻干燥,得到四种不同中药掺杂的导电聚吡咯/中药复合水凝胶。
如图2所示,4种掺杂中药分子的水凝胶的实物图显示,容器瓶倒置之后,样品仍然在瓶底保持较好的形态,说明成胶效果良好。
实施例2
导电聚吡咯/中药复合水凝胶的抗菌效果测试。通过抑菌环来表征这种导电聚吡咯/中药复合水凝胶的抗菌效果。取100μL大肠杆菌悬浮液(106CFU/ml)均匀涂布在LB琼脂平板上,静置一段时间,将实施例1所得的掺杂黄芩苷的导电聚吡咯复合水凝胶(直径1cm)放置在琼脂板中间,在37℃培育箱中培育24h后取出观察结果。所得抗菌结果如图4,在水凝胶四周形成一个明显的抑菌圈,这说明导电聚吡咯/中药复合水凝胶具有显著的抗菌效果。
对比例1
中药分子在水凝胶形成中起到重要作用,中药分子与吡咯形成氢键网络,有利于水凝胶的形成。如制备过程中无中药分子,水凝胶溃散难以成胶。具体地如下:
(1)取冰块放置于泡沫箱中,以维持低温环境。
(2)溶液A的准备:移取85μL的吡咯单体加入到1ml的异丙醇溶液中,磁力搅拌使其混合均匀。低温保存以待使用。
(3)溶液B的准备:称取0.274g过硫酸铵粉末加入到2ml去离子水中,在室温下磁力搅拌,待溶解完全后放入上述泡沫箱中,低温保存以待使用。
(4)用移液枪先后取70μL溶液A和140μL溶液B,加入到圆形模板中,搅拌10秒,静置1分钟。混合液迅速变黑,是吡咯氧化的结果。反应1小时后,具有类似的凝胶状态,但是非常脆弱,去除模板过程中溃散,且不断有水渗出,说明保水性较差。实物图如图5所示。由此可见,中药有利于成胶,提高聚吡咯的成胶性能。
对比例2
反应过程中,温度控制非常重要。在低温下,吡咯缓慢聚合,吡咯纳米结构缓慢生长,相互作用,相互之间形成纳米多孔结构,有利于保水,最终形成水凝胶。温度升高,吡咯聚合较快,形成比较独立的大尺寸纳米颗粒,分散在溶液中,相互之间的作用较弱,不能形成稳定的水凝胶。通过如下对比例得以佐证。
(1)溶液配制及反应都在室温下(25℃)进行。溶液A的准备:移取85μL的吡咯单体加入到1ml的异丙醇溶液中,磁力搅拌使其混合均匀。再称取0.03g中药(分别为黄芩苷、黄连素、姜黄素和人参皂苷)粉末溶于上述溶液,在室温下磁力搅拌,充分溶解。
(2)溶液B的准备:称取0.274g过硫酸铵粉末加入到2ml去离子水中,在室温下磁力搅拌,充分溶解。
(3)用移液枪先后取70μL溶液A和140μL溶液B,加入到圆形模板中,搅拌10秒,溶液迅速变黑。静置1小时后,仅有部分成胶,反应器中大部分仍然是比较黑色的溶液。实物图如图5所示。因此,在常温下,即使添加了各种中药分子,聚吡咯仍然难以形成水凝胶。
对比例3
(1)取冰块放置于泡沫箱中,以维持低温环境。
(2)溶液A的准备:移取85μL的吡咯单体加入到1ml的去离子水中,磁力搅拌使其混合均匀。低温保存以待使用。
(3)溶液B的准备:称取0.274g过硫酸铵粉末加入到2ml去离子水中,磁力搅拌使其混合均匀。再称取0.03g中药(分别为黄芩苷、黄连素、姜黄素和人参皂苷)粉末溶于上述溶液,在室温下磁力搅拌,待溶解完全后放入上述泡沫箱中,低温保存以待使用。
(4)用移液枪先后取70μL溶液A和140μL溶液B,加入到圆形模板中,搅拌10秒,静置1分钟,溶液迅速变黑,形成具有类似胶状结构的产物,但非常脆弱,去除模板过程中胶状产物溃散。实物图如图5所示。由此证明反应过程中需要以异丙醇为溶剂,充分溶解吡咯单体,以形成稳定均匀的水凝胶。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (7)
1.一种导电聚吡咯/中药复合水凝胶的制备方法,其特征在于,包括以下步骤:
(1)将吡咯单体溶于异丙醇中,再加入中药粉末,得到吡咯混合溶液;
(2)0~8℃下,将吡咯混合溶液与氧化剂水溶液在模板中迅速混合,搅拌一段时间后,静置,得到含杂质的聚吡咯水凝胶膜,洗涤,干燥,得到导电聚吡咯/中药复合水凝胶;
步骤(1)所述中药粉末为黄芩苷、黄连素、姜黄素和人参皂苷中的至少一种;步骤(1)所述吡咯单体和中药的比例为85μL:10~150mg;
步骤(2)所述洗涤指将含杂质的聚吡咯水凝胶膜依次在乙醇和水中浸泡,以去除多余的掺杂剂和副产物;
步骤(2)所述氧化剂水溶液中的氧化剂为过硫酸铵。
2.根据权利要求1所述一种导电聚吡咯/中药复合水凝胶的制备方法,其特征在于,步骤(1)所述吡咯单体和氧化剂的摩尔比为2:1~1:3。
3.根据权利要求1所述一种导电聚吡咯/中药复合水凝胶的制备方法,其特征在于,步骤(1)所述吡咯单体在异丙醇中的浓度为0.5~3mol/L;步骤(2)所述氧化剂水溶液的浓度为0.5~3mol/L。
4.根据权利要求1所述一种导电聚吡咯/中药复合水凝胶的制备方法,其特征在于,步骤(2)所述搅拌的时间为2~10秒,所述静置的时间为1~10分钟。
5.根据权利要求1所述一种导电聚吡咯/中药复合水凝胶的制备方法,其特征在于,步骤(2)所述干燥指在在30~120℃下真空干燥或者冷冻干燥。
6.权利要求1~5任一项所述方法制得的一种导电聚吡咯/中药复合水凝胶。
7.权利要求6所述一种导电聚吡咯/中药复合水凝胶在药物制备中的应用。
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