CN110409059A - 甲基丙烯酸二甲氨基乙酯增强的丙烯酰化pgs纳米纤维膜的制备方法 - Google Patents
甲基丙烯酸二甲氨基乙酯增强的丙烯酰化pgs纳米纤维膜的制备方法 Download PDFInfo
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Abstract
本发明公开了甲基丙烯酸二甲氨基乙酯增强的丙烯酰化PGS纳米纤维膜材料的制备及应用,本发明用于生物组织工程支架材料。该材料采用丙烯酰化PGS与DMAEMA为原料,制备方法是首先对聚癸二酸甘油酯进行改性,再PGS预聚物上接入双键(PGS‑A),通过将PGS‑A与DMAEMA单体混合,再聚乳酸助纺剂的作用下电纺丝制备纳米纤维,最后通过光聚合使PGS‑A/DMAEMA纤维固化成型。本发明将静电纺丝与光聚合技术相结合工艺简单、易控制,制备的纳米纤维膜材料比表面积大,柔韧性好,拉伸强度高,在增强PGS纳米纤维支架材料有重要的作用。
Description
技术领域
本发明属于生物医用组织工程领域,具体涉及甲基丙烯酸二甲氨基乙酯(DMAEMA)增强的丙烯酰化PGS纳米纤维膜的制备。
背景技术
组织工程支架材料是指能与组织活体细胞结合并能植入生物体的不同组织,并根据具体替代组织具备的功能的材料。为了使种子细胞增殖和分化,需要提供一个由生物材料所构成的细胞支架,支架材料相当于人工细胞外基质。
生物可降解聚合物在生物工程的各个领域具有巨大的潜力,如组织工程、药物输送,以及细胞微囊化等。天然细胞外基质(ECM),一种柔软、坚韧和弹性的蛋白质网络,为组织和器官提供机械稳定性和结构完整性。因此,一种柔软的可生物降解的弹性体可以从相对较大的变形中恢复过来,这有利于保持植入物的正常功能,而不会对宿主产生机械刺激。此外,这种替代天然细胞外基质的生物可降解材料还要具有很好的生物相容性、细胞亲和性等。被广泛研究的主要有水凝胶、弹性蛋白肽及聚羟基脂肪酸酯(PHA)等。
光聚合是自由基聚合的一种。单体分子借光的引发(或用光敏剂)活化成自由基而进行的连锁聚合。光引发剂吸收适当波长及强度的光能,发生光物理过程至其某一激发态,该激发态能量大于断裂键所需能量,产生初级活性种,通常为自由基,生成活性中心(自由基或离子)而引发单体聚合。
近年来,光聚合技术在生物医用中有着重要的作用。其中,大部分的水凝胶支架材料通过光聚合技术制备,较传统的聚合方式,光聚合具有效率高、反应条件温和、易控制等特点。因此,光聚合技术应用于组织工程支架材料,药物缓释材料,可注射水凝胶,细胞囊化等材料的制备。
聚癸二酸甘油酯(PGS)是一种韧性好、性价比高且具有良好细胞相容性的材料,其微观结构类似硫化胶,因为聚合物长链进行交联以及其氢键作用形成三维结构,所以与水凝胶相比,具有更强的韧性;与弹性蛋白肽相较具有无免疫性、无细胞毒性且价格便宜的优点;具有比PHA更大范围的形变恢复能力。甲基丙烯酸二甲氨基乙酯(DMAEMA)是一种常用的用于光聚合的单体,具有良好的亲水性,黏合性和热固化性能,由于PGS为一种类似硫化胶的如热塑性弹性体,在静电纺丝过程中往往需要增强材料来提高纤维的强度,我们选用聚乳酸PLA作为助纺剂并且起到支撑PGS纤维的作用,去掉助纺剂PLA后,PGS不能很好地保持纤维的形貌。
因此,我们通过将PGS丙烯酰化改性后,加入DMAEMA,通过光聚合技术,使得在单体聚合后,材料可以保持纤维的形貌,从而达到增强纤维的目的。并且提高纤维的亲水性,粘附性,将其应用于体内湿润表面。
发明内容
本发明的目的是针对PGS材料在组织工程中存在的强度问题,本发明提供一种甲基丙烯酸二甲氨基乙酯增强的丙烯酰化PGS纳米纤维膜的制备方法,本发明利用静电纺丝与光聚合技术相结合的方法,制备得到甲基丙烯酸二甲氨基乙酯增强的丙烯酰化PGS纳米纤维膜材料。
本发明采用的技术方案如下:
甲基丙烯酸二甲氨基乙酯增强的丙烯酰化PGS纳米纤维膜的制备方法,所述方法包括以下步骤:
(1)丙烯酰化PGS的制备方法:将PGS预聚物溶于二氯甲烷溶剂中,在上述溶液中加入12.026g三乙胺,后将0.01wt%的对羟基苯甲醚加入到上述溶液中,室温下搅拌,将一定量丙烯酰氯逐滴地加入溶液中,反应12h;利用乙酸乙酯沉淀过滤,并用稀盐酸洗涤后干燥,得丙烯酰化PGS,记为:PGS-A,低温下储存;
(2)电纺纳米纤维:将PGS-A与DMAEMA和以一定比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和一定量的助纺剂PLA,将溶液混合均匀后加入注射器中,通过施加高压电场,在滚筒接收器上收集纳米纤维;
(3)将得到的纳米纤维置于紫外灯下照射一段时间,后将纤维在室温下放置12h。
作为优选,所述步骤(1)中PGS与丙烯酰氯的质量比为5:3,丙烯酰氯/DCM的质量分数为15-30%。
作为优选,所述步骤(2)中PGS-A与DMAEMA的比例为1:1、2:1、1:2或4:1,PLA的浓度为8-15%。
作为优选,所述步骤(2)中电纺环境温度为25℃,湿度为20%,高压电源输出电压为20KV,针头流速为0.6mL/h,接收装置与喷丝口之间距离为20cm。
作为优选,所述步骤(3)中照射时间为5-20min。
甲基丙烯酸二甲氨基乙酯(DMAEMA)增强的丙烯酰化PGS纳米纤维膜的应用,作为生物医用材料,在组织工程中,通过应力应变曲线来表征纤维膜的机械强度,通过在体外细胞实验和体内活体实验进行测试。机械强度的测试中,利用拉力机来得到纤维膜的杨氏模量和断裂伸长率;在体外实验中,将细胞接种到纤维膜上,检测细胞黏附、迁移与增殖情况;在体内实验中,测试材料在体内炎症反应以及组织生长情况。
本发明的甲基丙烯酸二甲氨基乙酯(DMAEMA)增强的丙烯酰化PGS纳米纤维膜材料在组织工程中的应用,与之前的相关文献报道相比,具有以下优点:
(1)通过静电纺丝与光聚合技术相结合,方法简单,反应条件温和,易控制;
(2)鉴于PGS不能在静电场中喷射形成纤维,通过加入助纺剂,可以使得PGS具有纤维形态,增加材料的比表面积;
(3)将PGS改性之后,与DMAEMA材料进行复合,通过光聚合技术,使得PGS与DMAEMA交联,从而提高纤维的机械强度,从而改善PGS支架材料的拉伸性能;PGS是一种具有很好细胞相容性的材料,并且可生物降解,降解产生的废物可由人体代谢排出。
附图说明
图1为本发明所述静电纺丝实验简易装置图;
图2为本发明对PGS改性的红外光谱图;
图3为本发明对PGS改性的核磁氢谱图;
图4为本发明电纺制备的纤维膜材料的扫描电镜图;
图5为本发明纤维膜的拉伸强度和断裂伸长率。
具体实施方式
丙烯酰化PGS的制备实施例:
将PGS预聚物溶于二氯甲烷溶剂中,在上述溶液中加入一定质量的三乙胺,后将0.01wt%的对羟基苯甲醚加入到上述溶液中,室温下搅拌,将一定量丙烯酰氯逐滴地加入溶液中,反应12h;利用乙酸乙酯沉淀过滤,并用稀盐酸洗涤后干燥,得丙烯酰化PGS,记为:PGS-A,低温下储存;其红外光谱图如图2所示,核磁氢谱图如图3所示,
其中,PGS与丙烯酰氯的质量比为5:3,丙烯酰氯/DCM的质量分数为15-30%。
实施例1
将PGS-A与DMAEMA和以1:1的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和8wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;其中所使用的的静电纺丝实验简易装置图如图1所示,所获得的纤维膜材料的扫描电镜图如图4所示,
将收集的纤维膜在紫外光下照射5min,后再室温下放置12h,以充分发挥残余溶剂。
实施例2
将PGS-A与DMAEMA和以1:2的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和8wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射5min,后再室温下放置12h,以充分发挥残余溶剂。
实施例3
将PGS-A与DMAEMA和以2:1的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和8wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射5min,后再室温下放置12h,以充分发挥残余溶剂。
实施例4
将PGS-A与DMAEMA和以4:1的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和8wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射5min,后再室温下放置12h,以充分发挥残余溶剂。
实施例5
将PGS-A与DMAEMA和以1:1的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和8wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射10min,后再室温下放置12h,以充分发挥残余溶剂。
实施例6
将PGS-A与DMAEMA和以2:1的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和10wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射10min,后再室温下放置12h,以充分发挥残余溶剂。
实施例7
将PGS-A与DMAEMA和以4:1的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和10wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射10min,后再室温下放置12h,以充分发挥残余溶剂。
实施例8
将PGS-A与DMAEMA和以1:2的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和15wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射15min,后再室温下放置12h,以充分发挥残余溶剂。
实施例9
将PGS-A与DMAEMA和以1:4的比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和8wt%的助纺剂PLA,将溶液混合均匀后加入注射器中,连接到同轴针头上,在高压电设置为18KV,接收距离为20cm,流速为1mL/h的条件下静电纺丝,在滚筒接收器上收集纤维,滚筒转速为500rpm;
将收集的纤维膜在紫外光下照射10min,后再室温下放置12h,以充分发挥残余溶剂。
纤维膜的拉伸强度和断裂伸长率的测定
1)将电纺纤维膜分为两组,交联组和未交联组,将材料裁剪成相同规格(长:30mm,宽:10mm,厚:0.3mm)的样条,每组包括3个样条,放在万能试验机上进行测试,并记录拉伸强度和断裂伸长率的数据。
Claims (5)
1.甲基丙烯酸二甲氨基乙酯增强的丙烯酰化PGS纳米纤维膜的制备方法,其特征在于所述方法包括以下步骤:
(1)丙烯酰化PGS的制备方法:将PGS预聚物溶于二氯甲烷溶剂中,在上述溶液中加入12.026g三乙胺,后将0.01wt%的对羟基苯甲醚加入到上述溶液中,室温下搅拌,将一定量丙烯酰氯逐滴地加入溶液中,反应12h;利用乙酸乙酯沉淀过滤,并用稀盐酸洗涤后干燥,得丙烯酰化PGS,记为:PGS-A,低温下储存;
(2)电纺纳米纤维:将PGS-A与DMAEMA和以一定比例混合溶于二氯甲烷溶液中,再在上述溶液中加入1wt%光引发剂2959和一定量的助纺剂PLA,将溶液混合均匀后加入注射器中,通过施加高压电场,在滚筒接收器上收集纳米纤维;
(3)将得到的纳米纤维置于紫外灯下照射一段时间,后将纤维在室温下放置12h。
2.根据权利要求1所述的制备方法,其特征在于:所述步骤(1)中PGS与丙烯酰氯的质量比为5:3,丙烯酰氯在二氯甲烷溶剂中的质量分数为15-30%。
3.根据权利要求1所述的制备方法,其特征在于:所述步骤(2)中PGS-A与DMAEMA的比例为1:1、2:1、1:2或4:1,PLA的浓度为8-15%。
4.根据权利要求1所述的制备方法,其特征在于:所述步骤(2)中电纺环境温度为25℃,湿度为20%,高压电源输出电压为20KV,针头流速为0.6mL/h,接收装置与喷丝口之间距离为20cm。
5.根据权利要求1所述的制备方法,其特征在于:所述步骤(3)中照射时间为5-20min。
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