CN107185055B - 一种医用镁合金的表面改性方法 - Google Patents
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Abstract
本发明公开了一种医用镁合金的表面改性方法,首先对医用镁合金进行表面化学处理,然后自组装固定氨基硅烷分子,最后将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面,从而构建多功能的生物活性表面,同时提高材料的耐生理腐蚀性能。采用本发明的方法对医用镁合金进行表面改性,不仅可以提高镁合金的耐生理腐蚀性能,而且可以赋予材料良好的血液相容性和促内皮细胞生长性能,为医用镁合金在血管内植入材料或器械(如血管支架)领域的应用奠定良好的基础。
Description
技术领域
本发明涉及生物材料的技术领域,具体涉及一种医用镁合金的表面改性方法。
背景技术
冠状动脉粥样硬化性心脏病(常简称为冠心病)是冠状动脉发生粥样硬化病变而引起血管管腔狭窄或阻塞,造成心肌缺血、缺氧或坏死的心脏病。血管支架植入是目前治疗由于血管狭窄引发的冠心病的临床主要方法。目前用于血管支架制备的材料主要有不锈钢、镍钛合金、钴铬合金、铂铱合金等,但这些材料均为惰性材料,植入后将作为异物永久存留在体内,会不同程度地引发炎症、血栓形成、血管内膜增生等问题,从而导致支架内再狭窄。尽管各种表面改性技术以及药物涂层支架的应用在一定程度上降低了不可降解支架植入后的风险,但其临床应用效果尤其是长期应用效果仍然不尽满意。
镁合金材料具有良好的力学性能、可生物降解性能以及降解产物对人体无毒等特点,在心血管支架方面具有巨大的应用潜力,但是,镁在复杂体内生理环境下降解过快以及由于植入后血液成分及内皮细胞功能改变导致的表面血栓形成、内皮功能紊乱等问题常常导致植入失败。由于镁合金的腐蚀行为与生物相容性都与镁合金的表面性质密切相关,表面改性是目前同时提高镁合金耐蚀性能和生物相容性的有效方法。目前的表面改性方法主要有表面化学处理、表面合金化、表面热处理、微弧氧化、阳极氧化、制备表面覆盖层、等离子体处理等方法,但是这些方法很难同时提高镁合金的耐生理腐蚀性能、血液相容性以及促内皮细胞生长性能。
发明内容
本发明的目的在于:克服现有技术的不足,提供一种医用镁合金的表面改性方法,通过该方法可以构建一种具有多功能特性的镁合金表面,并显著提升镁合金在生理条件下的耐蚀性能和生物相容性,提高材料及其器械的植入成功率。
本发明所采取的技术方案是:
一种医用镁合金的表面改性方法,包括以下步骤:
1)首先对镁合金表面进行表面化学处理;
2)然后在经过化学处理后的镁合金表面自组装固定氨基硅烷分子;
3)最后将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面,得多具有良好耐蚀性能的具有多功能生物活性的镁合金生物材料。
本发明进一步改进方案是,所述步骤1)中,表面化学处理方法为:
1.1)将镁合金进行抛光、清洗;
1.2)将抛光清洗后的镁合金浸没到温度在50~90℃范围内的氢氧化钠和磷酸钠的混合溶液中处理15~60min。
本发明更进一步改进方案是,所述步骤1.2)中,所述氢氧化钠和磷酸钠混合溶液中的氢氧化钠(NaOH)的浓度在20~50 g/L 的范围内,十二水磷酸钠(Na3PO4·12H2O)的浓度在5~10 g/L 的范围内。
本发明更进一步改进方案是,所述步骤2)中,自组装固定氨基硅烷分子的方法为:
将步骤1)中的化学处理镁合金浸没到浓度在10~50mM范围内的氨基硅烷分子溶液中自组装反应12~24小时。
本发明更进一步改进方案是,所述氨基硅烷为氨丙基三甲氧基硅烷或氨丙基三乙氧基硅烷。
本发明更进一步改进方案是,所述步骤3)中,将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面的方法为:
3.1)将步骤2)中得到的镁合金材料首先浸没到聚乙二醇二羧酸、1-(3-二甲基氨基丙基 )-3-乙基碳二亚胺(EDC)及N-羟基丁二酰亚胺(NHS)的混合溶液中,充分反应4~12小时;
3.2)清洗干燥后浸没到纤连蛋白溶液中或纤连蛋白和肝素的混合溶液中继续反应4~12小时。
本发明更进一步改进方案是,所述步骤3.1)中,所述聚乙二醇二羧酸、EDC及NHS的混合溶液中,聚乙二醇二羧酸的浓度在1~10 mg/mL的范围内,EDC的浓度在5~20mM的范围内,NHS的浓度在5~20mM的范围内。
本发明更进一步改进方案是,所述步骤3.2)中,纤连蛋白的浓度在10µg~1mg/mL的范围内,肝素的浓度在1~10mg/mL的范围内。
本发明的有益效果在于:
第一、本发明的一种医用镁合金的表面改性方法,采用表面化学处理结合表面生物固定来同时提高镁合金的耐生理腐蚀性能、血液相容性和赋予材料促内皮细胞生长能力。
第二、本发明的一种医用镁合金的表面改性方法,本方法将具有抗生物污染的聚乙二醇分子、优异血液相容性的肝素分子以及细胞外基质蛋白-纤连蛋白固定在镁合金表面,可以赋予镁合金良好的抗生物污染能力、优异的血液相容性和促内皮愈合性能。
第三、本发明的一种医用镁合金的表面改性方法,本发明采用化学处理在镁合金表面首先形成耐蚀转化层,首先提高镁合金的耐蚀性能,从而使后续的自组装表面改性以及生物分子固定成为可能,有助于提高表面生物分子的固定量。
第四、本发明的一种医用镁合金的表面改性方法,本发明采用的表面自组装及聚乙二醇固定并不降低镁合金的耐蚀性能,反而进一步提高了镁合金的耐蚀性能。
附图说明:
图1为生物材料多功能生物活性表面构建的基本反应步骤示意图。
图中包括以下步骤:
(1)镁合金表面化学处理;
(2)镁合金自组装表面改性;
(3)镁合金表面接枝聚乙二醇;
(4)镁合金表面接枝纤连蛋白;
(5)镁合金表面接枝纤连蛋白/肝素复合物。
图2为镁合金表面改性后的动电位极化曲线测量结果图。
图3为镁合金表面改性后材料的溶血率柱状图。
图4为镁合金表面改性后内皮细胞粘附实验结果图。
具体实施方式:
如图1可知,本发明包括以下步骤:
1)首先对镁合金表面进行表面化学处理;
2)然后在经过化学处理后的镁合金表面自组装固定氨基硅烷分子;
3)最后将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面,得多具有良好耐蚀性能的具有多功能生物活性的镁合金生物材料。
所述步骤1)中,表面化学处理方法为:
1.1)将镁合金进行抛光、清洗;
1.2)将抛光清洗后的镁合金浸没到温度为75℃的氢氧化钠和磷酸钠的混合溶液中处理40min。
所述步骤1.2)中,所述氢氧化钠和磷酸钠混合溶液中的NaOH的浓度30 g/L,Na3PO4·12H2O的浓度为8 g/L。
所述步骤2)中,自组装固定氨基硅烷分子的方法为:
将步骤1)中的化学处理镁合金浸没到浓度为30mM的氨基硅烷分子溶液中自组装反应16小时。
所述氨基硅烷为氨丙基三甲氧基硅烷或氨丙基三乙氧基硅烷。
所述步骤3)中,将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面的方法为:
3.1)将步骤2)中得到的镁合金材料首先浸没到聚乙二醇二羧酸、EDC及NHS的混合溶液中,充分反应10小时;
3.2)清洗干燥后浸没到纤连蛋白溶液中或纤连蛋白和肝素的混合溶液中继续反应9小时。
所述步骤3.1)中,所述聚乙二醇二羧酸、EDC及NHS的混合溶液中,聚乙二醇二羧酸的浓度为7 mg/mL,EDC的浓度15mM,NHS的浓度为12mM。
所述步骤3.2)中,纤连蛋白的浓度为370µg/mL,肝素的浓度为6mg/mL。
由图2可知,镁合金化学处理后,腐蚀电流显著减小,表明化学处理显著提高了材料的耐蚀性能;自组装及接枝聚乙二醇后,腐蚀电流进一步减小,表明耐蚀性进一步提高。
由图3可知,未改性镁合金的溶血率高达50%以上,而接枝聚乙二醇或聚乙二醇和纤连蛋白-肝素复合物的材料,溶血率降低到5%以内,表明表面改性显著提升了材料的抗凝血性能。
由图4 可知,接枝聚乙二醇阻止了内皮细胞的粘附,而接枝纤连蛋白和纤连蛋白-肝素复合物的材料表面表现出显著的促内皮细胞粘附和生长性能。
Claims (7)
1.一种医用镁合金的表面改性方法,其特征在于包括以下步骤:
1)首先对镁合金表面进行表面化学处理;
2)然后在经过化学处理后的镁合金表面自组装固定氨基硅烷分子;
3)最后将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面,得多具有良好耐蚀性能的具有多功能生物活性的镁合金生物材料;
将聚乙二醇、纤连蛋白以及肝素依次固定在材料表面的方法为:
3.1)将步骤2)中得到的镁合金材料首先浸没到聚乙二醇二羧酸、1-(3-二甲基氨基丙基)-3-乙基碳二亚胺及N-羟基丁二酰亚胺的混合溶液中,充分反应4~12小时;
3.2)清洗干燥后浸没到纤连蛋白和肝素的混合溶液中继续反应4~12小时。
2.如权利要求1所述的一种医用镁合金的表面改性方法,其特征在于:所述步骤1)中,表面化学处理方法为:
1 .1)将镁合金进行抛光、清洗;
1.2)将抛光清洗后的镁合金浸没到温度在50~90℃范围内的氢氧化钠和磷酸钠的混合溶液中处理15~60min。
3.如权利要求2所述的一种医用镁合金的表面改性方法,其特征在于:所述步骤1 .2)中,所述氢氧化钠和磷酸钠混合溶液中的氢氧化钠的浓度在20~50 g/L 的范围内,十二水磷酸钠的浓度在5~10 g/L 的范围内。
4.如权利要求1所述的一种医用镁合金的表面改性方法,其特征在于:所述步骤2)中,自组装固定氨基硅烷分子的方法为:将步骤1)中的化学处理镁合金浸没到浓度在10~50mM范围内的氨基硅烷分子溶液中自组装反应12~24小时。
5.如权利要求4所述的一种医用镁合金的表面改性方法,其特征在于:所述氨基硅烷为氨丙基三甲氧基硅烷或氨丙基三乙氧基硅烷。
6.如权利要求1所述的一种医用镁合金的表面改性方法,其特征在于:所述步骤3 .1)中,所述聚乙二醇二羧酸、1-(3-二甲基氨基丙基)-3-乙基碳二亚胺及N-羟基丁二酰亚胺的混合溶液中,聚乙二醇二羧酸的浓度在1~10 mg/mL的范围内,1-(3-二甲基氨基丙基)-3-乙基碳二亚胺的浓度在5~20mM的范围内,N-羟基丁二酰亚胺的浓度在5~20mM的范围内。
7.如权利要求1所述的一种医用镁合金的表面改性方法,其特征在于:所述步骤3 .2)中,纤连蛋白的浓度在10µg~1mg/mL的范围内,肝素的浓度在1~10mg/mL的范围内。
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