CN111021056A - 聚己内酯/聚乳酸纳米纤维膜接枝白藜芦醇的制备方法 - Google Patents

聚己内酯/聚乳酸纳米纤维膜接枝白藜芦醇的制备方法 Download PDF

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CN111021056A
CN111021056A CN201811171425.3A CN201811171425A CN111021056A CN 111021056 A CN111021056 A CN 111021056A CN 201811171425 A CN201811171425 A CN 201811171425A CN 111021056 A CN111021056 A CN 111021056A
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polycaprolactone
polylactic acid
nanofiber membrane
resveratrol
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宋晓峰
张雪
王磊
王艳贺
夏文龙
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Changchun University of Technology
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Changchun University of Technology
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    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/152—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
    • D—TEXTILES; PAPER
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    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
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    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
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Abstract

本发明是一种在聚己内酯/聚乳酸纳米纤维膜上接枝白藜芦醇的制备方法。本文将所有的端羧基的聚己内酯和聚乳酸在静电纺丝条件下制备纳米纤维膜，真空干燥。之后纳米纤维膜进行预处理，在PBS中浸泡，得所需纤维膜。最后纤维膜与单体在黑暗下进行反应，通过表征证明了产物的合成。

Description

聚己内酯/聚乳酸纳米纤维膜接枝白藜芦醇的制备方法
技术领域
本发明涉及一种在纳米纤维膜上接枝单体的制备方法，属于高分子载药领域。
背景技术
随着高分子的功能化应用，将其利用于载药领域是现在发展趋势。由于药物自身缺陷以及使用方法的局限性，改善药物的缺陷以及拓展使用条件，对于药物的使用具有重要意义。药物使用包括口服，注射，以及外敷等，但单体药物的外敷需要借助一定的条件，因此本文根据白藜芦醇（RES）分解快以及增加作用到病灶部位的研究，研究了将药物单体共价接枝到纳米纤维膜聚己内酯/聚乳酸(PCL/PLLA)上的制备方法。
发明内容
本发明是在聚己内酯/聚乳酸纳米纤维膜上接枝白藜芦醇的制备方法。本文中的所有聚己内酯均为端羧化之后的。首先通过静电纺丝制备聚己内酯/聚乳酸的纳米纤维膜，真空干燥。之后将纳米纤维膜在PBS中进行浸泡，得所需纤维膜，最后将纤维膜与白藜芦醇单体在室温，黑暗条件下，加入催化剂进行接枝。
附图说明：
图一 聚己内酯/聚乳酸-白藜芦醇纳米纤维膜的外貌示意图。
图二 聚己内酯/聚乳酸-白藜芦醇纳米纤维膜的红外核磁谱图。
具体实施方式
具体实验案例步骤如下：
（1）制备聚己内酯/聚乳酸纳米纤维膜。将20/80的上述共混物通过静电纺丝，制备纳米纤维膜。之后真空干燥48h，保存备用。
（2）纳米纤维膜的预处理。将制备的纳米纤维膜浸泡在PBS中，为下一步的反应提供更加有利条件。
（3）纳米纤维膜共价接枝白藜芦醇。将处理后的纳米纤维膜和白藜芦醇在4-二甲氨基吡啶(DMAP), 1-乙基-(-3-二甲氨基丙基)碳酰二亚胺盐酸盐(EDC)的条件下进行共价接枝。
最终产物表征
载药纤维膜的形貌图如图一：
接枝之前纤维表面光滑，纤维直径均匀，为1.3μm左右(左图)。接枝后，纤维直径粗细变得不均匀，在0.5-2.7μm，结构更为复杂(右图)。
载药纤维膜的结构红外核磁分析如图二：
在红外谱图中，接枝后的纤维膜的特征峰有1758cm-1的羰基碳，1183cm-1的C-O伸缩振动键。1587cm-1和1510cm-1为白藜芦醇单体苯环上的C=C键的伸缩振动，在接枝后谱图的1509cm-1中可观察到。同时芳香族化合物上的C-H面外弯曲振动755cm-1也可被观察到（左图）。在核磁谱图中，聚乳酸的特征峰出现在图中的h(1.58ppm)和i(5.17ppm)处。聚己内酯的特征峰出现在a(1.38ppm),b(1.65ppm), c(2.30ppm), e(4.04ppm),f(4.08ppm)处。原料白藜芦醇两个羟基相邻的CH（a）的质子峰由6.11ppm偏移至6.17ppm。这些结果表明白藜芦醇已接枝到聚己内酯/聚乳酸纳米纤维膜上（右图）。

Claims (1)

1.本发明是在聚己内酯/聚乳酸纳米纤维膜上接枝白藜芦醇的制备方法，本文中所用的聚己内酯均为端羧基化的，特征在于：（1）通过静电纺丝制备20/80的聚己内酯/聚乳酸纳米纤维膜，电压7kv，距离15cm，6ml，纺丝速度1ml/h，溶剂氯仿（2）将上述纤维膜在PBS中进行浸泡，过夜，之后进行干燥备用（3）按聚己内酯和白藜芦醇摩尔比1：6进行投料，在DMAP，EDC催化条件下，黑暗条件下进行膜上的接枝反应，反应时间24小时，结束后用乙醇进行浸泡，水冲洗，最后真空干燥。
CN201811171425.3A 2018-10-09 2018-10-09 聚己内酯/聚乳酸纳米纤维膜接枝白藜芦醇的制备方法 Pending CN111021056A (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101302303A (zh) * 2007-05-08 2008-11-12 中国科学院化学研究所 表面接枝改性的可生物降解及吸收的聚酯超细纤维膜及制法和装置与膜的用途
CN105754122A (zh) * 2016-04-25 2016-07-13 苏州大学张家港工业技术研究院 一种亲水性聚己内酯薄膜的制备方法
CN106693072A (zh) * 2016-12-30 2017-05-24 北京化工大学 一种感染响应型引导组织再生膜的制备方法
CN108359088A (zh) * 2018-04-10 2018-08-03 长春工业大学 一种星型聚己内酯-白藜芦醇聚合物的制备方法

Patent Citations (4)

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CN101302303A (zh) * 2007-05-08 2008-11-12 中国科学院化学研究所 表面接枝改性的可生物降解及吸收的聚酯超细纤维膜及制法和装置与膜的用途
CN105754122A (zh) * 2016-04-25 2016-07-13 苏州大学张家港工业技术研究院 一种亲水性聚己内酯薄膜的制备方法
CN106693072A (zh) * 2016-12-30 2017-05-24 北京化工大学 一种感染响应型引导组织再生膜的制备方法
CN108359088A (zh) * 2018-04-10 2018-08-03 长春工业大学 一种星型聚己内酯-白藜芦醇聚合物的制备方法

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刘保健等: "聚乳酸/聚己内酯共混膜的结晶机理", 《高分子材料科学与工程》 *
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