CN116355258A - 基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法 - Google Patents
基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,首先将壳聚糖和增塑剂为基质材料通过铸膜‑挥发法制备壳聚糖膜,再将壳聚糖膜浸渍在含有可反应性官能团的羧甲基纤维素钠溶液中2‑12 h,然后滴加金属离子溶液,使负载有羧甲基纤维素钠和金属离子的壳聚糖膜置于两片玻璃片之间,于25‑60℃反应1‑12 h即可;本发明制备工艺简单,通过在壳聚糖膜上负载羧甲基纤维素钠水凝胶实现具有双层结构的烧伤敷料,利用壳聚糖的杀菌,促愈合以及镇痛性能以及羧甲基纤维素钠水凝胶为烧伤创面提供湿润环境,以此协同作用促进烧伤创面愈合,从而有望为烧伤患者和烧伤后的管理带来福音。
Description
技术领域
本发明属于生物医学材料技术领域,具体涉及一种基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法。
背景技术
烧伤会导致严重的人体损害,而这一切的损害都来源于烧伤对皮肤屏障作用的破坏。因此,在对烧伤的治疗中,寻求一种适宜的烧伤敷料来控制伤口感染并起到促进创面愈合的作用,在参与伤口护理与康复的过程是必须的。理想的烧伤敷料应具有多重特性:(1)吸收多余渗液,保持伤口环境湿润,利于坏死组织和纤维蛋白的溶解;(2)贴附于健康皮肤但不与新生肉芽组织粘连,避免更换敷料时的再次损伤;(3)不增加伤口感染的几率;(4)保持、促进各种生物活性因子或药物的释放;(5)加速肉芽组织与再上皮化的形成速度。
传统的烧伤敷料主要包括普通的纱布,脱脂棉和棉垫等。但是其存在诸多局限性,如难以维持创面湿润,纤维成分易发生脱落发生异物反应,敷料被浸透时易侵入病原体,敷料网眼中易贯穿新生肉芽组织使换药时造成组织损伤,换药难度高等。一些新型烧伤功能敷料因其能有效加速创面愈合的性能,而受到广大研究者们的青睐。水凝胶类敷料具有可紧密贴合非规整伤口,营造湿润环境的同时减少病原体入侵的概率,可吸收伤口渗出液等优异性能,使其作为生物相容性材料在治疗领域具有广泛的应用前景。如羧甲基纤维素钠水凝胶具有优异的防粘连和吸液性能,但单一组分的水凝胶敷料无法满足以上理想烧伤敷料的所有特性,往往需要对其功能化满足其特定的应用需求。如在水凝胶上通过物理方法负载AgNPs使其具有优异抗菌性能,但是AgNPs的安全性一直备受质疑;水凝胶也可通过化学方法修饰含抗菌性能的季铵盐官能团,但是该改性方法比较复杂,不适合于大规模化生产。同时研究者也有将两种组分的高分子材料复合制备水凝胶,但两种高分子材料进行复合往往面临结构不相容,导致均匀性不好,难以充分发挥和利用这些材料的优点。
发明内容
为了解决上述问题,本发明提供一种基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法。首先通过铸膜-挥发法制备壳聚糖薄膜,进一步通过浸渍法负载含反应性官能团的羧甲基纤维素钠,通过与金属离子交联形成羧甲基纤维素钠水凝胶。壳聚糖/羧甲基纤维素钠水凝胶烧伤敷料具有双层结构,通过协同作用可充分发挥壳聚糖的抑菌,防粘连,促愈合及镇痛性能以及羧甲基纤维素钠水凝胶的吸液性能等。
本发明采用的技术方案为:
一种基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,包括以下步骤:
(1)将壳聚糖加入酸性溶剂中,于室温下搅拌0.5-4h,再加入增塑剂,混合均匀后制备成铸膜液,再将铸膜液倒入培养皿中, 用pH调节剂调节pH为5.5-7.5,置于35-60℃干燥箱中2-12h,取出后用去离子水洗涤,烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入到含有反应性官能团的羧甲基纤维素钠水溶液中2-12h,取出并置于玻璃板上,继续向壳聚糖膜上滴加金属离子水溶液,直至膜表面上浸满金属离子溶液,再盖上一片玻璃板,稍微用力按压玻璃板,使溶液铺展均匀及壳聚糖膜平铺整齐,最后置于25-60℃下反应1-12h即得烧伤辅料。
所述的步骤(1)中壳聚糖:增塑剂:酸性溶剂的质量比为1:0.02-0.15:10-50。
所述的步骤(1)中的壳聚糖为市售的羧甲基壳聚糖、羟乙基壳聚糖和羟丙基壳聚糖中的一种或两种以上。
所述的步骤(1)中的酸性溶剂为乙酸、盐酸和磷酸的一种或两种以上,酸性溶剂的质量分数为0.5%-5%。
所述的步骤(1)中的增塑剂为甘油、蔗糖、山梨醇和聚乙二醇的一种或两种以上。
所述的步骤(1)中的pH调节剂为氨水和氢氧化钠的一种或两种。
所述的步骤(2)中含有反应性官能团的羧甲基纤维素钠:金属离子:溶剂的质量比为:1:0.05-0.2:20-40。
所述的步骤(2)中含有反应性官能团的羧甲基纤维素钠为含醛基的羧甲基纤维素钠,其质量分数为0.5%-10%。
所述的步骤(2)中金属离子为铝离子、锌离子、钙离子和银离子的一种或两种以上,金属离子水溶液的质量分数为0.5%-8%。
本发明的有益效果是:本发明制备工艺简单,原料成本低,在壳聚糖膜上构建羧甲基纤维素钠水凝胶制备具有双层结构的烧伤敷料,由于羧甲基纤维素钠水凝胶本身具有一定的粘性,易于负载到壳聚糖膜上;此外,由于羧甲基纤维素钠含有可反应性的醛基,可与壳聚糖上的氨基进行点击反应,进一步有利于羧甲基纤维素钠水凝胶在壳聚糖膜上的稳定性。羧甲基纤维素钠水凝胶能为烧伤场面提供湿润环境,可有效防止粘连及促进创面愈合,且羧甲基纤维素钠水凝胶具有优异的吸液性能,其三维网络结构中的水能为烧伤起到一定的降温作用;此外,壳聚糖具有抑菌性能,良好的止血及促愈合性能,可有效防止烧伤创面感染。本发明制备的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料可充分利用壳聚糖和羧甲基纤维素钠的水凝胶的各自优点,为烧伤创面如I度尤其是较难处理的深II度烧伤创面提供新的治疗选择。
附图说明
图1为本发明的烧伤辅料的主视图。
图2为本发明的烧伤辅料的侧面剖视图。
图中,1、羧甲基纤维素钠水凝胶,2、壳聚糖膜。
具体实施方式
以下通过优选实施例对本发明进一步详细说明,但本发明的保护范围并不局限于此。
一种基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,包括以下步骤:
(1)将壳聚糖加入酸性溶剂中,于室温下搅拌0.5-4h,再加入增塑剂,混合均匀后制备成铸膜液,再将铸膜液倒入培养皿中, 用pH调节剂调节pH为5.5-7.5,置于35-60℃干燥箱中2-12h,取出后用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入到含有反应性官能团的羧甲基纤维素钠水溶液中2-12h,取出并置于玻璃板上,继续往壳聚糖膜上滴加金属离子水溶液,直至膜表面上浸满金属离子溶液,再盖上一片玻璃板,稍微用力按压玻璃板,使溶液铺展均匀及壳聚糖膜平铺整齐,最后置于25-60℃下反应1-12h即得烧伤辅料。
所述的步骤(1)中壳聚糖:增塑剂:酸性溶剂的质量比为1:0.02-0.15:10-50。
所述的步骤(1)中的壳聚糖为市售的羧甲基壳聚糖、羟乙基壳聚糖和羟丙基壳聚糖中的一种或两种以上。
所述的步骤(1)中的酸性溶剂为乙酸、盐酸和磷酸的一种或两种以上,酸性溶剂的质量分数为0.5%-5%。
所述的步骤(1)中的增塑剂为甘油、蔗糖、山梨醇和聚乙二醇的一种或两种以上。
所述的步骤(1)中的pH调节剂为氨水和氢氧化钠的一种或两种。
所述的步骤(2)中含有反应性官能团的羧甲基纤维素钠:金属离子:溶剂的质量比为:1:0.05-0.2:20-40。这里的溶剂指的是水溶剂。
所述的步骤(2)中含有反应性官能团的羧甲基纤维素钠为含醛基的羧甲基纤维素钠,其质量分数为0.5%-10%。
所述的步骤(2)中金属离子为铝离子、锌离子、钙离子和银离子的一种或两种以上,金属离子水溶液的质量分数为0.5%-8%。
最后制成的烧伤辅料结构如图1-图2所示,图中1为羧甲基纤维素钠水凝胶:主要功能用来吸收渗液;2为壳聚糖膜:主要功能是发挥其抑菌,防粘连,促愈合及镇痛性能等;使用时,壳聚糖膜的一面接触皮肤。
实施例1
(1)将3g羧甲基壳聚糖颗粒放入质量分数3wt%的50 mL的乙酸溶液中,机械搅拌1h使壳聚糖颗粒完全溶解,加入0.1g甘油,搅拌均匀后制成铸膜液,将铸膜液倒入培养皿中,用氢氧化钠溶液调节其pH为7.0,并置于35 ℃的烘箱中12 h,取出后用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入2wt%的含醛基的羧甲基纤维素钠溶液2 h,取出并置于玻璃板上,往壳聚糖膜上滴加1wt%的氯化钙溶液,直至膜表面铺满氯化钙溶液,再盖上一个玻璃板,用适当的力按压使使溶液铺展均匀及壳聚糖膜平铺整齐;置于30℃温度下反应2 h,即得烧伤辅料成品。
实施例2
(1)将5g羧甲基壳聚糖颗粒放入质量分数1 wt%的60 mL的乙酸溶液中,机械搅拌0.5h使壳聚糖颗粒完全溶解,加入0.5g甘油,搅拌均匀后制成铸膜液,将铸膜液倒入培养皿中,并用氢氧化钠溶液调节其pH为6.5,并置于50 ℃的烘箱中12h,取出用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入4wt%的含醛基的羧甲基纤维素钠溶液中6h,取出并置于玻璃板上,往壳聚糖膜上滴加0.5wt%的氯化锌溶液,直至膜表面铺满氯化锌溶液,再盖上一个玻璃板,用适当的力按压使使溶液铺展均匀及壳聚糖膜平铺整齐;置于50℃温度下反应4 h,即得烧伤辅料成品。
实施例3
(1)将6g羟丙基壳聚糖颗粒放入质量分数3wt%的60mL的乙酸溶液中,机械搅拌0.5h使壳聚糖颗粒完全溶解,加入0.6g甘油,搅拌均匀后制成铸膜液,将铸膜液倒入培养皿中,并用氢氧化钠溶液调节其pH为6.0,并置于60 ℃的烘箱中6h,取出用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入1wt%的含醛基的羧甲基纤维素钠溶液中4 h,取出并置于玻璃板上,往壳聚糖膜上滴加3wt%的氯化铝溶液,直至膜表面铺满氯化铝溶液,再盖上一个玻璃板,用适当的力按压使使溶液铺展均匀及壳聚糖膜平铺整齐;置于40℃温度下反应2 h,即得烧伤辅料成品。
实施例4
(1)将1g羟丙基壳聚糖颗粒放入质量分数1 wt%的10 mL的乙酸溶液中,机械搅拌1h使壳聚糖颗粒完全溶解,加入0.15g甘油,搅拌均匀后制成铸膜液,将铸膜液倒入培养皿中,并用氢氧化钠溶液调节其pH为7.0,并置于55 ℃的烘箱中2h,取出用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入5wt%的含醛基的羧甲基纤维素钠溶液中8 h,取出并置于玻璃板上,往壳聚糖膜上滴加4wt%的氯化钙溶液,直至膜表面铺满氯化钙溶液,再盖上一个玻璃板,用适当的力按压使使溶液铺展均匀及壳聚糖膜平铺整齐;置于50℃温度下反应1 h,即得烧伤辅料成品。
实施例5
(1)将6g羟乙基壳聚糖颗粒放入质量分数1 wt%的100 mL的乙酸溶液中,机械搅拌3.5 h使壳聚糖颗粒完全溶解,加入0.5g甘油,搅拌均匀后制成铸膜液,将铸膜液倒入培养皿中,并用氢氧化钠溶液调节其pH为6.5,并置于50 ℃的烘箱中10 h,取出用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入2wt%的含醛基的羧甲基纤维素钠溶液中3 h,取出并置于玻璃板上,往壳聚糖膜上滴加2wt%的硝酸银溶液,直至膜表面铺满硝酸银溶液,再盖上一个玻璃板,用适当的力按压使使溶液铺展均匀及壳聚糖膜平铺整齐;置于45℃温度下反应1.5 h,即得烧伤辅料成品。
实施例6
(1)将2g羧甲基壳聚糖颗粒放入质量分数3 wt%的35 mL的乙酸溶液中,机械搅拌2h使壳聚糖颗粒完全溶解,加入0.1g甘油,搅拌均匀后制成铸膜液,将铸膜液倒入培养皿中,并用氢氧化钠溶液调节其pH为7.0,并置于35 ℃的烘箱中12h,取出用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入1wt%的含醛基的羧甲基纤维素钠溶液中6 h,取出并置于玻璃板上,往壳聚糖膜上滴加1wt%的氯化钙溶液,直至膜表面铺满氯化钙溶液,再盖上一个玻璃板,用适当的力按压使使溶液铺展均匀及壳聚糖膜平铺整齐;置于30℃温度下反应1 h,即得烧伤辅料成品。
Claims (9)
1.一种基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于,包括以下步骤:
(1)将壳聚糖加入酸性溶剂中,于室温下搅拌0.5-4h,再加入增塑剂,混合均匀后制备成铸膜液,再将铸膜液倒入培养皿中, 用pH调节剂调节pH为5.5-7.5,置于35-60℃干燥箱中2-12h,取出后用去离子水洗涤,再烘干即得壳聚糖膜;
(2)将壳聚糖膜浸入到含有反应性官能团的羧甲基纤维素钠水溶液中2-12h,取出并置于玻璃板上,继续往壳聚糖膜上滴加金属离子水溶液,直至膜表面上浸满金属离子溶液,再盖上一片玻璃板,按压玻璃板,使溶液铺展均匀及壳聚糖膜平铺整齐,最后置于25-60℃下反应1-12h即得烧伤辅料。
2.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(1)中壳聚糖:增塑剂:酸性溶剂的质量比为1:0.02-0.15:10-50。
3.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(1)中的壳聚糖为羧甲基壳聚糖、羟乙基壳聚糖和羟丙基壳聚糖中的一种或两种以上。
4.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(1)中的酸性溶剂为乙酸、盐酸和磷酸的一种或两种以上,酸性溶剂的质量分数为0.5%-5%。
5.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(1)中的增塑剂为甘油、蔗糖、山梨醇和聚乙二醇的一种或两种以上。
6.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(1)中的pH调节剂为氨水和氢氧化钠的一种或两种。
7.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(2)中含有反应性官能团的羧甲基纤维素钠:金属离子:溶剂的质量比为:1:0.05-0.2:20-40。
8.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(2)中含有反应性官能团的羧甲基纤维素钠为含醛基的羧甲基纤维素钠,其质量分数为0.5%-10%。
9.根据权利要求1所述的基于双层结构的壳聚糖膜和羧甲基纤维素钠水凝胶烧伤敷料的制备方法,其特征在于:所述的步骤(2)中金属离子为铝离子、锌离子、钙离子和银离子的一种或两种以上,金属离子水溶液的质量分数为0.5%-8%。
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