CN105801897A - 一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法 - Google Patents

一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法 Download PDF

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CN105801897A
CN105801897A CN201610285950.2A CN201610285950A CN105801897A CN 105801897 A CN105801897 A CN 105801897A CN 201610285950 A CN201610285950 A CN 201610285950A CN 105801897 A CN105801897 A CN 105801897A
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石畅
钮德宇
赵增辉
操莹
李雅瑜
沈佳丽
施冬健
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Jiangnan University
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Abstract

本发明提供一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法。本发明以聚乳酸(PLA)为基层材料，利用多巴胺(DA)的可黏附于多种材料表面的特性，在PLA表面涂覆一层聚多巴胺涂层改性得到PDA/PLA，再将预先制备的DA接枝透明质酸(HA‑DA)对改性得到的PDA/PLA基材进一步表面改性，得到HA‑DA/PDA/PLA复合材料。本发明制备所得的复合材料具有良好的降解性、细胞粘附性以及生物相容性，在骨修复、包装领域具有广阔的应用前景。

Description

一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法
技术领域
本发明涉及一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法，属于高分子材料和生物材料技术领域。
技术背景
随着骨组织工程材料的发展，研究者们发现细胞与材料之间的相互作用以及材料表面的性能对于骨缺损修复具有十分重要的影响。虽然高分子骨组织修复材料在应用中具有很多优势，但是仍存在一些缺陷，如：亲水性差，不利于细胞黏附、增殖和分化等，所以在临床医学领域，不仅要研发生物相容性良好的骨修复材料，还要研究如何改善材料表面与细胞、组织间的相互作用。
目前主要通过对骨组织修复材料进行表面改性来改善其各项性能。通过表面改性可以明显改善骨组织修复材料的表面亲水性，增强表面的粘结性，增加表面之间的相互作用，从而可以有效提高硬组织修复材料的细胞相容性，增加硬组织修复材料对于细胞的亲和性。现常用的表面改性方法有表面涂覆、接枝、等离子体改性等，其中涂覆法制备的涂覆层容易剥落，接枝改性其过程十分繁琐，等离子体处理则由于深度有限而受到限制。为此人们开始寻求更为简单有效的表面改性手段，来改善骨组织修复材料的表面粘接性能。随着生物仿生技术的快速发展，基于生物分子改性骨组织修复材料的研究逐渐成为人们关注的焦点。
透明质酸(HA)是糖胺聚糖中的一种，属于酸性粘多糖，其广泛分布于人体各部位，其中皮肤也含有大量的透明质酸.在机体内，透明质酸是一种多功能基质，显示出多种重要的生理功能，例如调节蛋白质，协助水电解质的扩散及运转，润滑关节，调节血管壁的通透性，促进伤口愈合等等.透明质酸具有特殊的保水作用，是目前发现的自然界中保湿性最好的物质，被称为理想的天然保湿因子.此外，透明质酸能与多种组织、细胞产生相互作用，因此其具有较好的组织、细胞黏附性能.透明质酸由于其具有独特理化性质和生理功能，已经在医学、生物材料方面得到了广泛应用.
本专利发明了一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法，利用聚多巴胺(DA)和透明质酸-多巴胺接枝物(HA-DA)涂敷改性涂覆聚乳酸(PLA)基体材料，制备得到PDA/HA细胞粘附性以及生物相容性，有望作为骨组织材料应用于生物医药领域。
发明内容
本发明的目的是提供一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法，得到的HA-DA/PDA/PLA复合材料具有良好的降解性、细胞粘附性以及生物相容性。
本发明的设计思路是：先利用多巴胺(DA)涂层对通过热压成型制备得到的聚乳酸(PLA)基体材料进行改性，再利用透明质酸-多巴胺接枝物(HA-DA)对其进行进一步涂敷改性，得到HA-DA/PDA/PLA复合材料。
本发明的技术方案为：将聚乳酸(PLA)进行热压成型得到聚合物基体材料；将多巴胺(DA)溶解在Tris·HCl缓冲液，然后将超纯水超声洗涤后的PLA基体材料浸入上述溶液中，在水浴恒温振荡器中于25℃下，反应24h后DA氧化自聚形成PDA并涂覆至PLA基材表面；在EDC和NHS的催化下，透明质酸(HA)与多巴胺(DA)通过酰胺化反应得到接枝物HA-DA；将HA-DA溶于盐酸溶液，最后将经超纯水超声洗涤的PDA/PLA浸入到HA-DA溶液中，在水浴恒温振荡器中25℃下表面涂覆12h；涂敷结束后取出基体材料，用超纯水超声洗涤，真空干燥24h，得到HA-DA/PDA/PLA复合材料。
聚乳酸的分子量为2.5×105；PLA基体材料热压成型的温度为175℃，压力为10MPa。
多巴胺在Tris·HCl缓冲液中的浓度都为1～5mg/mL；透明质酸(HA)与多巴胺(DA)的酰胺化反应中，两者的摩尔比HA:DA＝1:2～8，HA-DA溶液浓度为2～4mg/ml,盐酸溶液pH为2.0。
本发明的有益效果：本发明以生物基聚合物聚乳酸为原料。利用具有优异生物相容性的聚多巴胺(PDA)和透明质酸-多巴胺(HA-DA)对PLA基体材料进行表面改性，该种方法温和、简便，制备得到的复合材料具有良好的生物相容性生物可降解性、细胞粘附性，以及快速的矿化能力，这种复合材料具有修复骨组织的潜在应用价值。
附图说明
图1 HA-DA的紫外光谱(a)以及核磁共振图谱(b)
图2 HA-DA/DA改性前后PLA基体材料的SEM图
具体实施方式
实施例1、聚乳酸基体材料的制备
将PLA聚合物装入Φ8mm×1mm的不锈钢模具中，装好原料的模具在平板硫化机中175℃下预热5min，并在相同温度下，压力为10MPa正压5min，制备PLA基体材料。
实施例2、聚多巴胺表面改性材料的制备
将多巴胺盐酸盐溶解在10mM Tris·HCl缓冲液中(pH＝8.5)并使其浓度达到2mg/mL。把经超纯水超声洗涤的PLA基体材料浸入以上溶液中，在水浴恒温振荡器中25℃下反应24h进行表面涂覆；反应结束后取出PLA基体材料，用超纯水超声洗涤三到四次，40℃真空干燥24h。
实施例3、透明质酸-多巴胺(HA-DA)表面改性材料的制备
将透明质酸(HA)，多巴胺(DA)，EDC，NHS以1:2:2:4的投料比(摩尔比)进行酰胺化反应，得到HA-DA；将HA-DA溶解在盐酸溶液中(pH＝2.0)并使其浓度达到2mg/ml。最后把经超纯水超声洗涤的PDA/PLA基体材料浸入到以上溶液中，在水浴恒温振荡器中25℃下反应24h进行表面涂覆；反应结束后取出基体材料，用超纯水超声洗涤三到四次，40℃真空干燥24h。

Claims (5)

1.一种聚多巴胺/透明质酸改性涂覆聚乳酸膜的制备方法，其特征在于将聚乳酸(PLA)进行热压成型得到聚合物基体材料；将多巴胺(DA)溶解在Tris·HCl缓冲液，然后将超纯水超声洗涤后的PLA基体材料浸入上述溶液中，在水浴恒温振荡器中于25℃下，反应24h后DA氧化自聚形成PDA并涂覆至PLA基材表面；在EDC和NHS的催化下，透明质酸(HA)与多巴胺(DA)通过酰胺化反应得到接枝物HA-DA；将HA-DA溶于盐酸溶液，最后将经超纯水超声洗涤的PDA/PLA浸入到HA-DA溶液中，在水浴恒温振荡器中25℃下表面涂覆12h；涂敷结束后取出基体材料，用超纯水超声洗涤，真空干燥24h，得到HA-DA/PDA/PLA复合材料。
2.根据权利要求1所述的制备方法，其特征在于多巴胺在Tris·HCl缓冲液中的浓度都为1～5mg/mL，通过改变浓度，可以调控PDA层在PLA表面的涂覆厚度。
3.根据权利要求1所述的制备方法，其特征在于HA-DA接枝聚合物中HA和DA的摩尔比为HA:DA＝1:2～8。
4.根据权利要求1所述的制备方法，其特征在于HA-DA的浓度都为2～4mg/mL，盐酸溶液的pH为2.0。
5.根据权利要求1所述的制备方法，其特征在于PLA聚合物基体材料表面均匀沉积了HA-DA/PDA复合涂层，复合材料具有良好的降解性、细胞粘附性以及生物相容性，可以用作骨修复材料和包装材料。
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Cited By (9)

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CN106267337A (zh) * 2016-09-07 2017-01-04 江南大学 一种多巴胺基梯度功能材料的制备方法
CN107375196A (zh) * 2017-07-26 2017-11-24 暨南大学 一种含儿茶酚基天然多糖复合水凝胶载体及其制备方法
CN107376662A (zh) * 2017-09-15 2017-11-24 福州大学 一种具有良好亲水性能的pvdf/pda/ha复合膜
CN107383409A (zh) * 2017-07-26 2017-11-24 西南大学 一种制备促进血液相容性pdms基底的新方法
WO2018045905A1 (zh) * 2016-09-07 2018-03-15 江南大学 儿茶酚基改性生物大分子支架材料及其制备方法
CN110105733A (zh) * 2019-05-27 2019-08-09 江南大学 一种聚乳酸/聚乳酸接枝聚多巴胺复合材料的制备方法
CN112220777A (zh) * 2020-10-16 2021-01-15 北京大学口腔医学院 一种微环境响应型成骨细胞靶向载药纳米粒子及其制备方法和应用
CN113041409A (zh) * 2021-03-25 2021-06-29 西南交通大学 一种用于氧化应激环境下治疗的水凝胶载药涂层及其制备方法
CN115304775A (zh) * 2022-06-27 2022-11-08 天津大学 一种改性透明质酸修饰的胶原蛋白基质的制备方法

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CN106267337B (zh) * 2016-09-07 2019-11-19 江南大学 一种多巴胺基梯度功能材料的制备方法
US11384162B2 (en) 2016-09-07 2022-07-12 Jiangnan University Catechol group modified biomacromolecular scaffold material and preparation method thereof
WO2018045905A1 (zh) * 2016-09-07 2018-03-15 江南大学 儿茶酚基改性生物大分子支架材料及其制备方法
CN106267337A (zh) * 2016-09-07 2017-01-04 江南大学 一种多巴胺基梯度功能材料的制备方法
CN107375196A (zh) * 2017-07-26 2017-11-24 暨南大学 一种含儿茶酚基天然多糖复合水凝胶载体及其制备方法
CN107383409A (zh) * 2017-07-26 2017-11-24 西南大学 一种制备促进血液相容性pdms基底的新方法
CN107383409B (zh) * 2017-07-26 2020-05-26 西南大学 一种制备促进血液相容性pdms基底的方法
CN107376662B (zh) * 2017-09-15 2019-11-12 福州大学 一种具有良好亲水性能的pvdf/pda/ha复合膜
CN107376662A (zh) * 2017-09-15 2017-11-24 福州大学 一种具有良好亲水性能的pvdf/pda/ha复合膜
CN110105733A (zh) * 2019-05-27 2019-08-09 江南大学 一种聚乳酸/聚乳酸接枝聚多巴胺复合材料的制备方法
CN110105733B (zh) * 2019-05-27 2020-06-19 江南大学 一种聚乳酸/聚乳酸接枝聚多巴胺复合材料的制备方法
CN112220777A (zh) * 2020-10-16 2021-01-15 北京大学口腔医学院 一种微环境响应型成骨细胞靶向载药纳米粒子及其制备方法和应用
CN113041409A (zh) * 2021-03-25 2021-06-29 西南交通大学 一种用于氧化应激环境下治疗的水凝胶载药涂层及其制备方法
CN113041409B (zh) * 2021-03-25 2021-11-09 西南交通大学 一种用于氧化应激环境下治疗的水凝胶载药涂层及其制备方法
CN115304775A (zh) * 2022-06-27 2022-11-08 天津大学 一种改性透明质酸修饰的胶原蛋白基质的制备方法

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