CN106110380B - 一种氨基聚糖修饰硅藻基止血粉的制备方法 - Google Patents

一种氨基聚糖修饰硅藻基止血粉的制备方法 Download PDF

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CN106110380B
CN106110380B CN201610494583.7A CN201610494583A CN106110380B CN 106110380 B CN106110380 B CN 106110380B CN 201610494583 A CN201610494583 A CN 201610494583A CN 106110380 B CN106110380 B CN 106110380B
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冯超
李静
陈西广
孔明
程晓杰
刘雅
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Abstract

本发明公开了一种用于快速止血敷料的制备技术，即一种氨基聚糖修饰硅藻基止血粉的制备方法，以硅藻为基质材料，通过酸处理去除天然硅藻有机质，利用静电吸附和层层包被技术在硅藻外壳表面修饰氨基聚糖，真空干燥即得氨基聚糖修饰硅藻基止血粉，本发明产物具有快速止血和抑菌性能，所用原料均为生物可再生材料，天然无毒，试剂绿色环保，生产工艺简单，可用于急救、医疗以及战时伤员的紧急快速止血，具有良好的研究和开发利用前景。

Description

一种氨基聚糖修饰硅藻基止血粉的制备方法
技术领域
本发明属于生物材料领域的一种氨基聚糖修饰硅藻基止血粉的制备技术。
背景技术
战创伤救治是军事医学科学发展的重点研究方向，失血和感染是战伤造成死亡的重要原因，也是创伤急救以及外科手术经常遇到的难题。因此，开发有显著止血和抑菌效果的新型止血材料具有十分重要的科学和社会意义。硅藻是一类常见的单细胞微藻，在自然界中分布广泛，可以大规模人工养殖，经过简单纯化后可以获得形状规则、粒径均一的微米级硅藻外壳。硅藻外壳具有规则多孔结构，是天然的介孔硅基材料。硅藻外壳有很高的比表面积，能够大量吸附出血部位渗液，促进血小板和红细胞凝聚，促进血液凝固；同时，硅藻外壳表面富含大量的硅羟基基团，能够在血液辅因子HWK-kininogen和prekallikrein的协助下，引发凝血因子Ⅺ和Ⅻ的激活，加速凝血系统的启动。壳聚糖是一种天然氨基聚糖，因其具有良好的生物相容性、生物可降解性、血液及组织相容性，而广泛应用于生物医药领域。壳聚糖材料能够吸附血红细胞，促进血小板凝聚，促进血液凝固；同时，壳聚糖还具有广谱抑菌性。通过对壳聚糖进行修饰，如季铵化、巯基化、羧甲基化、羟丁基化、琥珀酰化，可以在提高壳聚糖的水溶性的同时，提高其抑菌性能。本发明以天然硅藻外壳为基质材料，表面修饰氨基聚糖材料，一方面，天然硅藻的介孔结构和活性表面能够大量吸附渗液，促进血液凝固；另一方面，其表面修饰的氨基聚糖材料能够在加快血液凝固的同时，抑制细菌生长，避免创面感染。
发明内容
本发明的目的是提供一种氨基聚糖修饰硅藻基止血粉的制备方法，以弥补已有技术的不足。
本发明以硅藻外壳为基质载体，通过酸处理、氨基聚糖包被合成目标产物即氨基聚糖修饰硅藻基止血粉，其具体步骤是：
（1）硅藻外壳纯化：将硅藻用筛绢过滤，置于30%过氧化氢和2 mol/L盐酸中，其中过氧化氢与盐酸的体积比为1 : 1，静置24小时，用500目筛绢再次过滤后分别用去离子水和无水乙醇洗涤三次，置于真空干燥箱中在35 ℃下过夜干燥后即得纯化的硅藻外壳；
（2）氨基聚糖包被：将纯化后硅藻外壳置于氨基聚糖水溶液中，室温下搅拌3小时，过滤，重新置于氨基聚糖水溶液中，室温下搅拌3小时后，离心弃上清，分别用去离子水和无水乙醇洗涤沉淀三次，置于真空干燥箱中在35 ℃干燥24小时，即得氨基聚糖包被的硅藻外壳。
本发明具有操作简便、制备技术工艺简单以及制造成本低廉等优点，可以通过改变氨基聚糖浓度和种类改善本产品促凝血和抑菌性能，所形成的氨基聚糖修饰硅藻基止血粉为介孔刚性粉末，具有快速止血和抑菌性能，可以作为伤口敷料应用于战创止血和急救等领域，具有良好的开发应用潜力，以下结合附图和实施例对本发明做出进一步说明。
附图说明
图1为纯化后硅藻外壳扫描电镜照片。
图2为氨基聚糖修饰硅藻基止血粉扫描电镜照片。
具体实施方式
实施例1
配制10 mL浓度为10 mg/mL的季铵化壳聚糖溶液，加入200 mg纯化硅藻外壳，将反应体系置于磁力搅拌器上搅拌，速度为500 rpm，反应温度为25 ℃，时间3小时，包被结束后过滤，再重复包被一次，然后分别用去离子水和无水乙醇洗涤三次。置于真空干燥箱中在35℃干燥24小时，即得季铵化壳聚糖包被的硅藻外壳。
实施例2
配制20 mL浓度为10 mg/mL的羧甲基壳聚糖溶液，加入400 mg纯化硅藻外壳，将反应体系置于磁力搅拌器上搅拌，速度为500 rpm,反应温度为25 ℃，时间3小时，包被结束后过滤，再重复包被一次，然后分别用去离子水和无水乙醇洗涤三次。置于真空干燥箱中在35℃干燥24小时，即得羧甲基壳聚糖包被的硅藻外壳。
实施例3
配制10 mL浓度为5 mg/mL的羟丁基壳聚糖溶液，加入200 mg纯化硅藻外壳，将反应体系置于磁力搅拌器上搅拌，速度为500 rpm，反应温度为25 ℃，时间3小时，包被结束后过滤，再重复包被一次。然后分别用去离子水和无水乙醇洗涤三次。置于真空干燥箱中在35℃干燥24小时，即得羟丁基壳聚糖包被的硅藻外壳。

Claims (1)

1.一种氨基聚糖修饰硅藻基止血粉的制备方法，其特征在于以硅藻为基质材料，通过酸处理去除天然硅藻有机质，利用静电吸附和层层包被技术在硅藻外壳表面修饰氨基聚糖，真空干燥即得氨基聚糖修饰硅藻基止血粉，具体为：
（1）硅藻外壳纯化：将硅藻用筛绢过滤，置于30%过氧化氢和2 mol/L盐酸中，其中过氧化氢与盐酸的体积比为1 : 1，静置24小时，用500目筛绢再次过滤后分别用去离子水和无水乙醇洗涤三次，置于真空干燥箱中在35 ℃下过夜干燥后即得纯化的硅藻外壳；
（2）氨基聚糖包被：将纯化后硅藻外壳置于氨基聚糖水溶液中，所述氨基聚糖为：壳聚糖、羟丁基化壳聚糖、羟丙基壳聚糖、巯基化壳聚糖、季铵化壳聚糖、琥珀酰化壳聚糖或羧甲基化壳聚糖，其中壳聚糖、羟丁基化壳聚糖、羟丙基壳聚糖、巯基化壳聚糖水溶液浓度为1-5mg/mL；季铵化壳聚糖、琥珀酰化壳聚糖、羧甲基化壳聚糖水溶液浓度为1-10 mg/mL，其添加量为氨基聚糖与硅藻外壳的质量比为0.05 - 0.5 : 1，室温下搅拌3小时，过滤，重新置于氨基聚糖水溶液中，室温下搅拌3小时后，离心弃上清，分别用去离子水和无水乙醇洗涤沉淀三次，置于真空干燥箱中在35 ℃干燥24小时，即得氨基聚糖包被的硅藻外壳。
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