CN113046917A - 一种静电纺丝胶原膜及其制备方法 - Google Patents

一种静电纺丝胶原膜及其制备方法 Download PDF

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CN113046917A
CN113046917A CN202110169124.2A CN202110169124A CN113046917A CN 113046917 A CN113046917 A CN 113046917A CN 202110169124 A CN202110169124 A CN 202110169124A CN 113046917 A CN113046917 A CN 113046917A
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collagen
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electrostatic spinning
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陈卫英
陈真勇
黎云祥
杨在君
匙峰
邹建
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China West Normal University
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Abstract

本发明提供了一种静电纺丝胶原膜的制备方法，取胶原蛋白、乙酸和水混合得到纺丝溶液，进行静电纺丝即可；其中，胶原蛋白的质量分数为9‑10％，乙酸的质量分数为27‑37％。本发明还提供了制备的静电纺丝胶原膜及其用途。本发明方法简单方便、环境友好，制备的胶原膜外观良好、质地柔软，弹性模量高，具有较强机械性能，大大拓宽了胶原蛋白在组织工程及再生医学中的应用，具有良好的临床前景。

Description

一种静电纺丝胶原膜及其制备方法
技术领域
本发明属于医学材料领域，具体涉及一种静电纺丝胶原膜及其制备方法。
背景技术
胶原是哺乳动物体内含量最丰富的结构蛋白质。其中，I型胶原约占总胶原量的90％以上，因具有优异的生物相容性、降解性、无毒性、低免疫原性，非常适合作为医用生物材料来使用。实际应用中，I型胶原可加工成各种形态的生物医用材料，应用于组织工程支架、创伤敷料、口腔修复、药物传递系统、止血等生物医学领域。
静电纺丝(Electrostatic spinning)是制备纤维材料的一种新型方式，可使聚合物溶液在静电作用下进行喷射拉伸而获得纳米纤维，制成的纤维膜具有比表面积大，孔隙率高等特点。将胶原蛋白通过静电纺丝制成胶原膜，能很好地模仿细胞外基质的结构，在组织修复和促伤口愈合等领域有巨大的应用前景。
目前公认胶原蛋白静电纺丝的理想溶剂为六氟异丙醇(HFIP)，但它具有溶剂毒性和使胶原蛋白变性的缺点，往往会在一定程度上破坏胶原的三股螺旋结构。乙酸溶液能快速溶解胶原蛋白，且不易破坏胶原肽链，可考虑作为静电纺丝胶原膜的溶剂。但目前使用乙酸溶剂尝试制备胶原蛋白胶原膜的报道中，通常认为单独使用乙酸溶液为溶剂，纺丝时难以形成纤维，需要添加辅纺溶剂如聚氧化乙烯【李晓龙等，I型胶原蛋白纳米纤维膜的制备及结构表征[J]，食品与药品，2016(2)：83-86】；而Andrea Fiorani使用体积比为20％的乙酸，虽然制成了乙酸-胶原膜，但胶原膜的弹性模量仅为84±8MPa，力学强度差，应用范围受限【Fiorani A et al.Comparative performance of collagen nanofibers electrospunfrom different solvents and stabilized by different crosslinkers[J].J MaterSci Mater Med,2014,25(10):2313-2321.】。
因此，以乙酸溶液作为溶剂进行胶原蛋白静电纺丝仍需进一步改良。
发明内容
针对现有技术中的问题，本发明提供了一种具有良好机械性能的静电纺丝胶原膜及其制备方法。
本发明提供了一种静电纺丝胶原膜的制备方法，取胶原蛋白、乙酸和水混合得到纺丝溶液，进行静电纺丝即可；
其中，胶原蛋白的质量分数为9-10％，乙酸的质量分数为27-37％。
进一步地，所述胶原蛋白的质量分数为10％，乙酸的质量分数27-36％。
优选地，所述胶原蛋白的质量分数为10％，乙酸的质量分数36％。
本发明中，称取胶原蛋白时，是以胶原海绵重量来计，胶原蛋白重量分数也是以胶原海绵重量计。
其中，所述胶原蛋白为I型胶原蛋白。
其中，所述胶原蛋白来源于牛。
其中，所述静电纺丝的参数为：高压为50-80kV，接收距离为15-18cm。
其中，所述高压为65kV，接收距离为15cm，转子速度为3.0r/min。
其中，步骤如下：
(1)制备乙酸水溶液；
(2)将胶原蛋白与乙酸水溶液混合，进行静电纺丝即可。
本发明还提供了上述方法制备的静电纺丝胶原膜。
本发明还提供了上述静电纺丝胶原膜作为生物医用材料的用途。
本发明人通过大量实验研究发现，只有特定浓度的胶原与特定浓度的乙酸溶液配比，才能制备出平整光滑、力学性能优良的静电纺丝胶原膜。本发明方法简单方便，原料无毒性，制备的胶原膜外观良好、质地柔软，纤维平均直径为(305.19±119.67)nm，纤维与纤维间层次清晰、呈网状交错分布，弹性模量高，机械性能好，韧性好，易剪裁，方便进行临床操作。
本发明胶原膜具有良好的力学性能，大大拓宽了胶原蛋白在组织工程及再生医学中的应用，在骨缺损治疗、口腔颌面缺损修复领域大有作为；也可作为补片材料，例如作为人工硬脑膜补片，用于因颅脑、脊髓损伤、肿瘤及其他颅脑疾病引起的硬脑膜或脊膜缺损修补等；另外可应用于人工角膜、心血管支架等方面，临床应用前景广泛。
显然，根据本发明的上述内容，按照本领域的普通技术知识和惯用手段，在不脱离本发明上述基本技术思想前提下，还可以做出其它多种形式的修改、替换或变更。
以下通过实施例形式的具体实施方式，对本发明的上述内容再作进一步的详细说明。但不应将此理解为本发明上述主题的范围仅限于以下的实例。凡基于本发明上述内容所实现的技术均属于本发明的范围。
附图说明
图1静电纺丝胶原膜的外观；其中，图1A的溶剂为质量浓度40％的乙酸水溶剂；图1B的溶剂为质量浓度为30％的乙酸水溶剂。
图2.静电纺丝胶原膜的扫描电镜观察。
具体实施方式
下面以实施例作进一步说明，但本发明不局限于这些实施例。
本发明所用的实验试剂与仪器设备如下：
I型胶原海绵，成都达普医疗器械有限公司；冰乙酸，重庆茂业化学试剂有限公司；NSLAB200纳米蜘蛛丝静电纺丝仪，捷克ELmarco公司；ES-3038型磁力搅拌仪，上海越磁电子科技有限公司；万能试验机AG-5000G，日本岛津公司；AL-204型电子天平，瑞士MettlerToledo公司；冷冻真空干燥仪，上海一恒科学仪器有限公司。
实施例1本发明胶原膜的制备
制备方法如下：
(1)配制质量比为40％的乙酸水溶液；
(2)称取胶原蛋白，配制胶原浓度为10％(w/w)的乙酸-胶原混合纺丝溶液；
(3)在室温25±2℃，空气湿度40±2％条件下，利用磁力搅拌器将纺丝溶液混合均匀。利用ELmarco纳米蜘蛛丝静电纺丝仪进行静电纺丝，制作胶原膜。纺丝条件为：高压65kV，转子速度3.0r/min，接收距离15cm，用锡箔纸收集，得到胶原蛋白膜。
以下通过试验例具体说明本发明的有益效果：
试验例1本发明胶原膜制备方法的参数筛选
一、胶原-乙酸溶液的静电纺丝可纺性实验
配制不同浓度胶原-乙酸混合溶液：质量比为40％、30％、20％的乙酸水溶液；用电子天平称取胶原蛋白，再分别按质量比配制表1所示不同浓度的胶原-乙酸混合溶液。利用移液器取1mL不同浓度的胶原-乙酸混合溶液，利用ELmarco纳米蜘蛛丝静电纺丝仪对溶液进行静电纺丝可纺性实验。纺丝条件为：室温25±2℃，空气湿度40±2％，高压65kV，接收距离15cm。结果见表1。
表1.不同浓度胶原-乙酸混合溶液的可纺性
Figure BDA0002938367980000041
由表1可见：编号1和6，分别为40％、30％乙酸水溶液为溶剂，配制成胶原蛋白10％的混合溶液，在65KV高压下出丝均匀，具有可纺性。其余乙酸水溶液和胶原配比时，均可纺性差，部分混合溶液甚至无纺丝。
二、大量胶原-乙酸电纺溶液制备胶原膜验证
按照表1的可纺性实验结果，选择出丝和可纺性最好的胶原-乙酸混合溶液，进行进一步考察。
具体方法为：称量4.5g胶原蛋白，用相应的乙酸溶液进行溶解，配制成10％(w/w)的胶原-乙酸混合溶液。然后在室温25±2℃，空气湿度40±2％条件下，利用磁力搅拌器将胶原-乙酸混合液混合均匀。利用ELmarco纳米蜘蛛丝静电纺丝仪进行大量静电纺丝，制作胶原膜。纺丝条件为：高压65kV，转子速度3.0r/min，接收距离15cm，用锡箔纸收集，制备出静电纺丝胶原膜。利用冷冻真空干燥仪对胶原膜进行干燥24小时，并将干燥后的胶原膜(图1)置于4℃冰箱保存。
结果显示，当溶剂为30％乙酸水溶液，胶原质量分数为10％浓度时，制备的静电纺丝胶原膜呈乳白色，虽然膜表面整体平整光滑，但从外缘到内部均出现明显的凹陷，甚至是孔洞(图1B)。而且在整个纺丝过程中，均观察有小液滴飞升。
而当溶剂为40％乙酸水溶液，胶原质量分数为10％浓度时，仅在纺丝开始时，观察到些许小液滴伴随纺丝飞升，在纺丝进行三分钟后，不再有小液滴飞升。制备的静电纺丝胶原膜呈乳白色，膜表面平整光滑，除2个明显凹陷点外，无明显粗糙、颗粒感(图1A)。
因此，溶液为40％乙酸水溶液，制备的10％胶原乙酸混合溶液可纺性好，胶原膜外观最佳。
试验例2本发明胶原膜的力学性能考察
按照实施例1的方法进行静电纺丝，制备静电纺丝胶原膜。然后利用万能试验机对静电纺丝胶原膜进行单轴拉伸试验，检测其力学性能。
具体方法为：取静电纺丝胶原膜裁剪成3个长度30mm、宽10mm的样品(经测量其厚度为0.2mm)，每个样品在测试前预加载至0.1N以防止样品松弛，设置标距为30mm、拉伸速度为10mm/min，测定并记录拉伸弹性模量、拉伸强度以及断裂时的最大力，然后计算出不同样品相关参数平均值，结果见表2。
表2本发明胶原蛋白膜的力学特性
Figure BDA0002938367980000051
由表2可见：本发霉制备的静电纺丝胶原膜拉伸弹性模量为(749.22±107.72)MPa，弹性模量高，甚至超过以往报道的静电纺丝胶原混纺膜性能。进行力学实验得到胶原最大拉伸力平均值为21.92±3.03N，具有较强的机械性能。因此，本发明胶原蛋白膜的力学性能优良。
试验例3本发明胶原膜的纤维形貌观察
取实施例1方法制备的胶原蛋白膜，对纤维采用喷金处理，在扫描电镜下观察纤维形貌。由图2可见：该静电纺丝胶原膜纤维整体排列杂乱无序、呈网状交错分布、个别纤维上有点堆积，是由于电纺初期飞升的小液滴形成；纤维与纤维层次清晰明显、脉络整体清晰；纤维直径不等，个别纤维直径略大一些。利用Image J图像分析软件随机选取其中100条纤维测量直径，计算得到纤维平均直径为(305.19±119.67)nm。
本发明获得的胶原蛋白膜，纤维直径不等，层次明显，交错排列形成网状结构，纤维交错排列，大大提高了静电纺丝胶原膜的力学性能。
综上，本发明方法操作简单，制备的胶原膜弹性模量高，力学性能良好，可广泛应用于组织工程及再生医学方面，满足不同临床需求，具有良好的临床应用价值。

Claims (10)

1.一种静电纺丝胶原膜的制备方法，其特征在于：取胶原蛋白、乙酸和水混合得到纺丝溶液，进行静电纺丝即可；
其中，胶原蛋白的质量分数为9-10％，乙酸的质量分数为27-37％。
2.根据权利要求1所述的制备方法，其特征在于：所述胶原蛋白的质量分数为10％，乙酸的质量分数27-36％。
3.根据权利要求2所述的制备方法，其特征在于：所述胶原蛋白的质量分数为10％，乙酸的质量分数36％。
4.根据权利要求1-3任意一项所述的制备方法，其特征在于：所述胶原蛋白为I型胶原蛋白。
5.根据权利要求1-3任意一项所述的制备方法，其特征在于：所述胶原蛋白来源于牛。
6.根据权利要求1-5任意一项所述的制备方法，其特征在于：所述静电纺丝的参数为：高压为50-80kV，接收距离为15-18cm。
7.根据权利要求6所述的制备方法，其特征在于：所述高压为65kV，接收距离为15cm，转子速度为3.0r/min。
8.根据权利要求1-7任意一项所述的制备方法，其特征在于：步骤如下：
(1)制备乙酸水溶液；
(2)将胶原蛋白与乙酸水溶液混合，进行静电纺丝即可。
9.权利要求1-8任意一项方法制备的静电纺丝胶原膜。
10.权利要求9所述的静电纺丝胶原膜作为生物医用材料的用途。
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