CN106075532A - 一种壳聚糖无纺布及其制备方法与应用 - Google Patents

一种壳聚糖无纺布及其制备方法与应用 Download PDF

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CN106075532A
CN106075532A CN201610465546.3A CN201610465546A CN106075532A CN 106075532 A CN106075532 A CN 106075532A CN 201610465546 A CN201610465546 A CN 201610465546A CN 106075532 A CN106075532 A CN 106075532A
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邢桂英
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Abstract

本发明公开了一种壳聚糖无纺布及其制备方法与应用，其特征在于：以聚甲基丙烯酸为共纺高分子材料，与壳聚糖静电共纺制备壳聚糖超细纤维，然后将上述壳聚糖超细纤维通过高温交联，制备壳聚糖无纺布。本发明通过静电纺丝技术制备的壳聚糖无纺布，具有纤维细小，高度多孔性，高比表面积等特点，采用聚甲基丙烯酸同时作为共纺试剂和交联试剂，有效地提高壳聚糖的可纺性，利用N,N‑二甲基甲酰胺或二甲亚砜作为助溶剂提高无纺布中纳米纤维的形貌；交联后的壳聚糖无纺布表现出良好结构稳定性、耐溶剂性能、耐酸碱性能以及药物缓释性能；并且通过调节交联时间和温度还可以对药物缓释性能进行调节，从而扩展了壳聚糖无纺布的应用范围。

Description

一种壳聚糖无纺布及其制备方法与应用
技术领域:
本发明涉及一种微纳米级无纺布载药体系，具体涉及一种壳聚糖无纺布及其制备方法与应用。
背景技术：
甲壳素是从甲壳类动物如虾，昆虫，螃蟹等动物壳中萃取的一种天然聚合物，目前在自然界中的产量仅次于纤维素，而壳聚糖是甲壳素脱乙酰后的产物。壳聚糖具有良好的生物相容性和生物可降解性，在生物体可以降解为CO2和水，因此壳聚糖在生物医学、组织工程、药物缓释、细胞及酶的固定化、高分子膜材料等方面具有十分广泛的应用。
纳米材料具有极大的比表面积，可以使得药物组分能够得到很好的分散和固定，被认为是性能超群的药物载体材料。其中由静电纺丝制得的纳米级超细纤维具有比表面积高、孔隙率大、纤维结构可控、适易于高分子材料的微加工等优点，是一类优良的药物载体材料。由于壳聚糖仅溶于酸性溶液中，同时由于壳聚糖分子链上含有大量的氨基，在酸性溶液中质子化，从而使分子链相互排斥，最终导致纯粹壳聚糖的静电纺丝非常困难。目前只有少数文献报道了壳聚糖的静电纺丝，而且需要用到剧毒和腐蚀性的三氟乙酸作为溶剂或助溶剂（孙康，王丽平. 壳聚糖静电纺纳米纤维的制备和特点. 应用化学, 2011, 28: 123-130.）。因此目前常用的制备壳聚糖静电纺丝膜是采用和其它高分子进行共纺制备得到，如聚氧化乙烯，聚乙烯醇和聚交酯等．如天津大学袁晓燕等通过共纺制备的壳聚糖/聚氧化乙烯(聚乙烯醇)和聚α-羟基酸酯/壳聚糖等超细纤维形成的无纺布，具有吸水量大、降解速度可调控，细胞亲核性好等优点，可在组织领域得到应用 (袁小燕，张园园，段斌等，壳聚糖纳米超细纤维膜材料及其制备方法，中国专利，No. CN1569254；聚α-羟基酸酯/壳聚糖超细纤维杂化膜材料及其制备方法，中国专利，No. CN1569255)；Toshkova等通过静电纺丝的方法，将抗癌药阿霉素、壳聚糖和聚交酯制备成阿霉素无纺布，动物体内研究结果发现该无纺布对Graffi肿癌细胞表现出较高的毒性，动物的存活率得到提高、而且复发率也明显减小(Toshkova R, Manolova N, Gardeva E, Ignatova M et al, Antitumor activity ofquaternized chitason-based electrospun implants against Graffi myeloid tumor.International Journal of Pharmaceutics, 2010, 400: 221-223)。
发明内容:
本发明的第一方面目的是提供了一种具有良好溶剂稳定性和机械性能、耐酸碱的壳聚糖无纺布。
本发明采取的技术方案如下：
一种壳聚糖无纺布，其特征在于：以聚甲基丙烯酸为共纺高分子材料，与壳聚糖静电共纺制备壳聚糖超细纤维，然后将上述壳聚糖超细纤维通过高温交联，制备壳聚糖无纺布，该无纺布纤维平均直径为100 nm~500 nm。
本发明的第二方面目的是提供一种壳聚糖无纺布的制备方法，其特征在于，包括以下步骤：
（1）配制壳聚糖/聚甲基丙烯酸/药物溶液：
a): 配制壳聚糖溶液：将分子量为5～100 万的壳聚糖和分子量为0.5～20万的聚甲基丙烯酸溶于50～90 wt.%乙酸水溶液，60℃搅拌溶解得到7.5～15 wt.%的混合溶液；
b)：往步骤a配置的混合溶液中加入1-10wt.% 的N,N-二甲基甲酰胺或二甲亚砜溶剂，搅拌得到均匀溶液；
c)往步骤b配置的溶液中加入0.01-0.5 wt.%的水溶性药物，配置得壳聚糖/聚甲基丙烯酸/药物溶液；
所述的水溶性药物选自阿司匹林、水杨酸、左氧氟沙星、安乃近、头孢拉定、阿莫西林的任意一种，优选为水杨酸或左氧氟沙星。
（2）壳聚糖/聚甲基丙烯酸/药物溶液静电纺丝：
将步骤（1）配制的壳聚糖/聚甲基丙烯酸/药物溶液装入静电纺丝装置的注射器中，进行静电纺丝，得到壳聚糖超细纤维，其中：注射器嘴内径为0.7～1.2 mm，静电纺丝工艺条件为：电压为15 kV～30 kV、流量为0.5～1.5 mL/h、接收距离为10～25 cm；
（3）无纺布的交联：
将步骤（2）制备的壳聚糖超细纤维置于烘箱中，于150-250℃进行交联反应1 – 6 小时，得到壳聚糖无纺布。
优选地，将壳聚糖超细纤维在空气或氮气或氩气或真空条件下，于150~250℃进行交联反应1-6小时，得到壳聚糖无纺布。
上述制备得到的壳聚糖无纺布：纤维直径：100~500 nm；比表面积：1.2~10.0 m2/g；无纺布在50%乙酸溶液中48小时溶胀率小于500%；载药量：0 ~ 40 %。具有纤维细小、高度多孔性、高比表面积、结构稳定性、耐溶剂性能、耐酸碱性能、高载药量、药物缓释性能好等优点。
本发明的第三方面目的是提供了一种壳聚糖无纺布作为医用敷料的应用，本发明的壳聚糖无纺布作为医用敷料应用时，可有效控制药物的缓释性能。
本发明的有益效果如下：
1、本发明通过静电纺丝技术制备的壳聚糖无纺布，具有纤维细小，高度多孔性，高比表面积等特点，
2、采用聚甲基丙烯酸同时作为共纺试剂和交联试剂，有效地提高壳聚糖的可纺性，利用N,N-二甲基甲酰胺或二甲亚砜作为助溶剂提高无纺布中纳米纤维的形貌；
3、交联后的壳聚糖无纺布表现出良好结构稳定性、耐溶剂性能、耐酸碱性能以及药物缓释性能；并且通过调节交联时间和温度还可以对药物缓释性能进行调节，从而扩展了壳聚糖无纺布的应用范围。
以下结合附图和具体实施方式对本发明作进一步说明。
附图说明：
图1为实施例1制备的壳聚糖无纺布放大2000倍扫描电镜图；
图2为实施例1制备的壳聚糖无纺布50wt.%醋酸溶液中浸泡24小时后放大2000倍扫描电镜图；
图3为实施例2制备的壳聚糖无纺布放大2000倍扫描电镜图；
图4为实施例1和2制备的壳聚糖无纺布在PBS (pH = 7.4)缓冲溶液中的水杨酸释放结果；
图5 为实施例3制备的壳聚糖无纺布在PBS (pH = 7.4)缓冲溶液中的水杨酸释放结果。
具体实施方式:
实施例1：
取分子量为20万的壳聚糖 0.35g，分子量8 万聚甲基丙烯酸0.35g，60℃下溶于7.0g、65 wt.%的乙酸水溶液中，然后再加1.0 g的N,N-二甲基甲酰胺溶剂，搅拌溶解后，再加入0.035g水杨酸溶解，搅拌溶解，向带有内径为1.2mm平头针头的20mL注射器中注入纺丝溶液，将注射器固定在微量注射泵上，在距离针头15cm处放置金属接收屏；将针头与25 kV的高压直流电源相连，设定2.0 mL/h 流量进行静电纺丝，在20 h后接收屏收集到直径约为187 nm的壳聚糖超细纤维，然后在烘箱中180℃处理2 h，得到壳聚糖无纺布。
实施例2：
取分子量为20万的壳聚糖0.35g，2万聚甲基丙烯酸0.35g，60 ℃下溶于7.0g、65 wt.%的乙酸水溶液中，然后再加1.0 g的二甲亚砜，搅拌溶解后，再加入0.035 g水杨酸溶解，搅拌溶解。向带有内径为1.2 mm平头针头的20 mL注射器中注入纺丝溶液，将注射器固定在微量注射泵上，在距离针头15 cm处放置金属接收屏。将针头与25 kV的高压直流电源相连，设定2.0 mL/h 流量进行静电纺丝，在20 h后接收屏收集到直径约为457 nm的壳聚糖超细纤维；然后在烘箱中160℃处理2 h，得到壳聚糖无纺布。
实施例3、不同交联时间对缓释性能的影响。
制备方法同实施例1，区别在于：改变交联时间，分别在180℃交联1、2、6小时以研究其对壳聚糖无纺布的水杨酸缓释性能影响，检测结果如图5所示。缓释性能实验如下：将20 mg 壳聚糖无纺布置于100 mL PBS 溶液（pH=7.4）中，20℃恒温振荡，采用紫外光谱检测溶液在波长为295 nm处吸收峰（水杨酸紫外特征吸收峰）变化。
产品性能检验：
将实施例1～3制备的壳聚糖无纺布，分别进行电镜扫描、耐溶剂性能、药物缓释性能检测，统计结果如图1～图5所示。
1、电镜扫描：
如图1所示，实施例1制备的壳聚糖无纺布，具有纤维细小、高度多孔性、高比表面积等特点，聚甲基丙烯酸同时作为共纺试剂和交联试剂，有效地提高壳聚糖的可纺性，纤维直径：150~500 nm，比表面积：1.2~10.0 m2/g，无纺布的拉伸强度为11.2 MPa。
结合图3所示，实施例2以二甲基亚砜作为助溶剂，能大幅提高无纺布的纤维直径，因此，可以通过添加二甲亚砜调节无纺布的纤维直径。
2、耐溶剂性能：
如图2所示，交联后的壳聚糖无纺布表现出良好的结构稳定性、耐溶剂性能、耐酸碱性能；在50wt.%醋酸溶液中浸泡24小时后纤维结构无明显变化。
3、药物缓释性能：
如图4所示，实施例1、实施例2制备的壳聚糖无纺布，可以有效控制药物的释放性能。
如图5所示，通过调节交联时间和温度，可以对药物缓释性能进行调节，从而扩展了壳聚糖无纺布的应用范围，最佳工艺为交联温度180℃，交联时间6小时。

Claims (7)

1.一种壳聚糖无纺布，其特征在于：以聚甲基丙烯酸为共纺高分子材料，与壳聚糖静电共纺制备壳聚糖超细纤维，然后将上述壳聚糖超细纤维通过高温交联，制备壳聚糖无纺布。
2.根据权利要求1所述的一种壳聚糖无纺布，其特征在于：所述壳聚糖无纺布：纤维直径：100~500 nm；比表面积：1.2~10.0 m2/g；无纺布在50%乙酸溶液中48小时溶胀率小于500%；载药量：0 ~ 40 %。
3.一种壳聚糖无纺布的制备方法，其特征在于，包括以下步骤：
（1）配制壳聚糖/聚甲基丙烯酸/药物溶液：
a): 配制壳聚糖溶液：将分子量为5～100 万的壳聚糖和分子量为0.5～20万的聚甲基丙烯酸溶于50～90 wt.%乙酸水溶液，60℃搅拌溶解得到7.5～15 wt.%的混合溶液；
b)：往步骤a配置的混合溶液中加入1-10wt.% 的N,N-二甲基甲酰胺或二甲亚砜溶剂，搅拌得到均匀溶液；
c)往步骤b配置的溶液中加入0.01-0.5 wt.%的水溶性药物，配置得壳聚糖/聚甲基丙烯酸/药物溶液；
（2）壳聚糖/聚甲基丙烯酸/药物溶液静电纺丝：
将步骤（1）配制的壳聚糖/聚甲基丙烯酸/药物溶液装入静电纺丝装置的注射器中，进行静电纺丝，得到壳聚糖超细纤维，其中：注射器嘴内径为0.7～1.2 mm，静电纺丝工艺条件为：电压为15 kV～30 kV、流量为0.5～1.5 mL/h、接收距离为10～25 cm；
（3）无纺布的交联：
将步骤（2）制备的壳聚糖超细纤维置于烘箱中，于150-250 ℃进行交联反应1 – 6 小时，得到壳聚糖无纺布。
4.根据权利要求1所述的一种壳聚糖无纺布的制备方法，其特征在于：将壳聚糖超细纤维在空气或氮气或氩气或真空条件下，于150~250℃进行交联反应1-6小时，得到壳聚糖无纺布。
5.根据权利要求1所述的一种壳聚糖无纺布的制备方法，其特征在于：所述的水溶性药物选自阿司匹林、水杨酸、左氧氟沙星、安乃近、头孢拉定、阿莫西林的任意一种。
6.根据权利要求5所述的一种壳聚糖无纺布的制备方法，其特征在于：所述的水溶性药物为水杨酸或左氧氟沙星。
7.一种壳聚糖无纺布作为医用敷料的应用，其特征在于：所述壳聚糖无纺布作为医用敷料应用时，可有效控制药物的缓释性能。
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