CN107137776A - 一种海藻酸钠复合生物玻璃修复材料的制备方法 - Google Patents
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Abstract
一种海藻酸钠复合生物玻璃修复材料的制备方法,属于生物医药材料领域,包括:海藻酸钠溶液的制备、生物玻璃溶液的制备、静电纺丝制得修复材料。其中海藻酸钠可以改善材料的机械性能,生物玻璃可以改善材料的医药性能。本发明制得的修复材料具有良好的机械性能、组织修复性能及药物附着性。
Description
技术领域
本发明属于生物医药材料领域,尤其涉及一种海藻酸钠复合生物玻璃修复材料的制备方法。
背景技术
自发现生物玻璃至今,人们更多关注的是生物玻璃组份对生物活性的影响。纳米技术的兴起,使人们开始认识到结构对生物活性也有重要影响,更加注重于尺寸效应、微观精细结构对材料结构和性能的影响。从纳米尺寸出发研发设计的纳米生物玻璃、介孔生物玻璃更是备受国内外学者的关注。生物玻璃能激活细胞基因,有利于增强细胞的增殖与分化,具有骨诱导和骨传导的作用。但鉴于其无定形硅骨架的存在,生物玻璃仍呈现为无定形态,机械性能差,且药物附着性差,其在生物医药材料上的应用还有待进一步开发。
发明内容
为了解决现有技术中存在的问题,本发明提供了一种机械性能好,且具有优良的药物附着性的海藻酸钠复合生物玻璃修复材料的制备方法。
本发明采用以下技术方案:
一种海藻酸钠复合生物玻璃修复材料的制备方法,包括以下步骤:
步骤一:100g褐藻加入1000mL去离子水中,洗净后切成1cm×1cm的方块,以质量百分比10%加入到120mL质量浓度为1.5%的Na2CO3水溶液中,消化3h,再中和至pH为中性,以10倍体积水稀释消化液,搅拌后离心得到上清液,将上清液中加入5mg纤维素酶进行酶解反应1h,经柠檬酸缓冲液中和至中性,再加入125mL质量浓度为10%的CaCl2水溶液进行钙析,再加入质量浓度为3%的HCl酸化30min,生成褐藻酸凝块,滤去HCl后水洗至pH中性,加入褐藻酸凝块6倍体积的质量浓度为15%的NaCl进行离子交换脱钙,再加入体积浓度95%的乙醇析出絮状沉淀,经离心、烘干后即得海藻酸钠;
步骤二:将500mg海藻酸钠溶于100ml去离子水中,60℃水浴中溶解1h,磁力搅拌1000r/min,溶解1h,制成质量浓度0.5%的海藻酸钠溶液;
步骤三:将5g聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物溶于62g体积浓度为70%的乙醇溶液中,充分搅拌后,依次加入6g硅酸乙酯、0.7g磷酸三乙酯、1.5gCa(NO3)2·4H2O、1g0.5M盐酸溶液,得混合液;
步骤四:将混合液在室温下搅拌24h后静置,当溶液呈粘稠状溶液时,即制得生物玻璃溶液;
步骤五:将海藻酸钠溶液与生物玻璃溶液按质量比50:9混合均匀,使用超声波震荡对其进行分散,50℃条件下磁力搅拌1h,再在室温下继续搅拌8h,得到粘稠溶液置于与高压装置连接的医用针管中,通过静电纺丝制得修复材料,高压装置电压为20kV,将制得的材料在40℃下真空干燥。
优选的,步骤五中所述的医用针管的容量为20ml。
优选的,步骤五中所述的医用针管的针头固定在距离静电纺丝接收板20cm处。
本发明的有益效果在于:
1)海藻酸钠具有优良的生物相容性及机械性能,可降解性好,是很好的组织工程支架材料,此外海藻酸钠含有游离的羧基和羟基,性质活泼,容易与其他高分子物质相结合形成良好的复合材料。
2)生物玻璃具有良好的生物相容性,且具有组织修复的功能,能激活细胞基因,有利于增强细胞的增殖与分化,具有骨诱导和骨传导的作用。
3)海藻酸钠可以改善材料的机械性能,生物玻璃可以改善材料的医药性能。
4)采用静电纺丝技术制备的材料,具有良好的孔隙率,有利于药物的附着。
具体实施方式
下面结合实施例对本发明做进一步的描述。
实施例1
一种海藻酸钠复合生物玻璃修复材料的制备方法,包括以下步骤:
步骤一:100g褐藻加入1000mL去离子水中,洗净后切成1cm×1cm的方块,以质量百分比10%加入到120mL质量浓度为1.5%的Na2CO3水溶液中,消化3h,再中和至pH为中性,以10倍体积水稀释消化液,搅拌后离心得到上清液,将上清液中加入5mg纤维素酶进行酶解反应1h,经柠檬酸缓冲液中和至中性,再加入125mL质量浓度为10%的CaCl2水溶液进行钙析,再加入质量浓度为3%的HCl酸化30min,生成褐藻酸凝块,滤去HCl后水洗至pH中性,加入褐藻酸凝块6倍体积的质量浓度为15%的NaCl进行离子交换脱钙,再加入体积浓度95%的乙醇析出絮状沉淀,经离心、烘干后即得海藻酸钠;
步骤二:将500mg海藻酸钠溶于100ml去离子水中,60℃水浴中溶解1h,磁力搅拌1000r/min,溶解1h,制成质量浓度0.5%的海藻酸钠溶液;
步骤三:将5g聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物溶于62g体积浓度为70%的乙醇溶液中,充分搅拌后,依次加入6g硅酸乙酯、0.7g磷酸三乙酯、1.5gCa(NO3)2·4H2O、1g0.5M盐酸溶液,得混合液;
步骤四:将混合液在室温下搅拌24h后静置,当溶液呈粘稠状溶液时,即制得生物玻璃溶液;
步骤五:将海藻酸钠溶液与生物玻璃溶液按质量比50:9混合均匀,使用超声波震荡对其进行分散,50℃条件下磁力搅拌1h,再在室温下继续搅拌8h,得到粘稠溶液置于与高压装置连接的医用针管中,通过静电纺丝制得修复材料,高压装置电压为20kV,将制得的材料在40℃下真空干燥。
步骤五中所述的医用针管的容量为20ml,步骤五中所述的医用针管的针头固定在距离静电纺丝接收板20cm处。
Claims (3)
1.一种海藻酸钠复合生物玻璃修复材料的制备方法,其特征在于,包括以下步骤:
步骤一:100g褐藻加入1000mL去离子水中,洗净后切成1cm×1cm的方块,以质量百分比10%加入到120mL质量浓度为1.5%的Na2CO3水溶液中,消化3h,再中和至pH为中性,以10倍体积水稀释消化液,搅拌后离心得到上清液,将上清液中加入5mg纤维素酶进行酶解反应1h,经柠檬酸缓冲液中和至中性,再加入125mL质量浓度为10%的CaCl2水溶液进行钙析,再加入质量浓度为3%的HCl酸化30min,生成褐藻酸凝块,滤去HCl后水洗至pH中性,加入褐藻酸凝块6倍体积的质量浓度为15%的NaCl进行离子交换脱钙,再加入体积浓度95%的乙醇析出絮状沉淀,经离心、烘干后即得海藻酸钠;
步骤二:将500mg海藻酸钠溶于100ml去离子水中,60℃水浴中溶解1h,磁力搅拌1000r/min,溶解1h,制成质量浓度0.5%的海藻酸钠溶液;
步骤三:将5g聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物溶于62g体积浓度为70%的乙醇溶液中,充分搅拌后,依次加入6g硅酸乙酯、0.7g磷酸三乙酯、1.5gCa(NO3)2·4H2O、1g0.5M盐酸溶液,得混合液;
步骤四:将混合液在室温下搅拌24h后静置,当溶液呈粘稠状溶液时,即制得生物玻璃溶液;
步骤五:将海藻酸钠溶液与生物玻璃溶液按质量比50:9混合均匀,使用超声波震荡对其进行分散,50℃条件下磁力搅拌1h,再在室温下继续搅拌8h,得到粘稠溶液置于与高压装置连接的医用针管中,通过静电纺丝制得修复材料,高压装置电压为20kV,将制得的材料在40℃下真空干燥。
2.根据权利要求1所述的一种海藻酸钠复合生物玻璃修复材料的制备方法,其特征在于:步骤五中所述的医用针管的容量为20ml。
3.根据权利要求1所述的一种海藻酸钠复合生物玻璃修复材料的制备方法,其特征在于:步骤五中所述的医用针管的针头固定在距离静电纺丝接收板20cm处。
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