CN105477686B - 一种包覆黄腐酚的纳米纤维膜 - Google Patents

一种包覆黄腐酚的纳米纤维膜 Download PDF

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CN105477686B
CN105477686B CN201510849188.1A CN201510849188A CN105477686B CN 105477686 B CN105477686 B CN 105477686B CN 201510849188 A CN201510849188 A CN 201510849188A CN 105477686 B CN105477686 B CN 105477686B
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xanthohumol
fibrous membrane
nano fibrous
plla
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宋晓峰
乔天奎
宋平
蒋苏臣
郭慧玲
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Changchun University of Technology
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Abstract

本发明涉及一种包覆黄腐酚（Xanthohumol，Xn）的纳米纤维膜，纳米纤维膜中接枝纳米羟基磷灰石（HA‑g‑PLLA）的含量为5 wt%，黄腐酚的含量为5 wt%~20 wt%，将上述原料与生物可降解聚酯高分子（如聚丙交酯、聚乙交酯‑丙交酯共聚物）溶解于溶剂制成纺丝液，通过电纺丝制得包覆黄腐酚的载药纳米纤维膜。FTIR测试表明黄腐酚包封于纳米纤维；经SEM观察到纳米纤维膜的表面形貌；利用接触角分析仪测试了纳米纤维膜的亲水性的变化；通过药物体外释放实验绘制黄腐酚的释放曲线，可以调整各种组分的混合比例控制药物释放速率。其中加入的HA‑g‑PLLA增强了纤维膜的生物活性，有益于骨修复，而黄腐酚可以诱导骨髓间充质干细胞向成骨细胞的分化，同时还具有抗肿瘤，抗氧化，抗炎的作用。

Description

一种包覆黄腐酚的纳米纤维膜
技术领域
本发明属于骨修复材料领域，涉及一种包覆黄腐酚的载药纳米纤维膜、制备方法。
背景技术
黄腐酚是异戊烯基黄酮类化合物，广泛存在于啤酒花中的天然产物，它们以多方面的生理活性及独特的化学结构引起了国内外药学家的广泛兴趣。因其具有显著地抗癌、抗氧化特性，在医药研究领域渐渐得到重视。同时黄腐酚具有类似雌性激素的性质，对于成骨细胞的分化成熟具有一定的作用，可以用于调节更年期妇女的骨代谢平衡，改善的骨质量和骨密度，在骨修复领域具有非常大的应用潜力。
纳米羟基磷灰石与骨头的无机成分相似，可以增强骨细胞的黏附和活力，诱导新骨形成，因此，引入纳米羟基磷灰石可以提高聚酯类纳米纤维膜的生物活性，同时还能改善复合纳米纤维膜的相关性能。
静电纺丝加工的纳米纤维膜具有较高的孔隙率，高精细度、大比表面积、较好的均一性等优点，而且与天然的细胞间质具有类似的结构，有利于营养物质的透过，促进细胞的迁移和增殖，因此可用于临床治疗和组织工程。特别是可降解聚酯类的电纺纳米纤维膜，可在体内降解，不需要二次手术取出，减少了患者的痛苦和治疗费用。静电纺丝纳米纤维膜在骨修复和载药方面的应用研究已经非常广泛，将黄腐酚与纳米羟基磷灰石通过电纺丝成纳米纤维膜材料还从未见有报道。
发明内容
本发明目的是提供一种包覆黄腐酚纳米纤维膜材料。将黄腐酚与聚酯/ HA-g-PLLA材料一同溶解制得纺丝液，利用电纺丝法制备纳米纤维膜。在纳米纤维膜的形成过程中，黄腐酚均匀的分布在其中，该纤维具有良好的生物相容性和生物可降解性。
本发明中包覆黄腐酚的纳米纤维膜特征在于以生物可降解的聚酯为基体，经电纺丝制得聚酯/接枝纳米羟基磷灰石/黄腐酚的复合纳米纤维膜。其中聚酯的含量为90 ~ 75wt%，纳米羟基磷灰石的含量为5 wt%，黄腐酚的含量为5 ~ 20 wt%，用合适的溶剂溶解，磁力搅拌得到均匀的纺丝液，通过静电纺丝装置进制备包覆黄腐酚的纳米纤维膜材料。所述包覆黄腐酚的载药纳米纤维，其特征在于所述黄腐酚有效成分是黄腐酚，异黄腐酚，8-异戊烯基柚皮素中的一种或几种的混合物。所述的生物可降解聚酯为聚ε己内酯（PCL）、聚L-乳酸（PLLA）、聚乙交酯丙交酯（PLGA）中的一种或几种的混合物。所述的溶剂为三氯甲烷、二氯甲烷、甲苯、二甲苯、三氯甲烷/N，N-二甲基甲酰胺混合溶剂、二氯甲烷/N，N-二甲基甲酰胺混合溶剂中的一种。所述的静电纺丝装置的参数为纺丝电压5 ~ 20 kV，两极间距离为10~20 cm，纺丝液在喷丝口处的流速为0.3 ~1.5 mL/h。所述聚酯/ HA-g-PLLA /黄腐酚的电纺复合纳米纤维膜材料，其特征在于骨修复应用。
有益效果
(1) 黄腐酚具有多种药理活性和医疗效果，但是其性质不稳定，在受热，酸碱等情况下均会变性失去药用价值，电纺丝有利于保持黄腐酚的活性，实现药物缓释；
(2) 包覆黄腐酚的复合纳米纤维膜的加工工艺简单易行。
(3) 载有黄腐酚和HA-g-PLLA的纳米纤维膜有利于骨修复中的应用。
附图说明
图1包覆黄腐酚的纳米纤维及释放过程示意图。
图2为黄腐酚(a)、纯PLGA纤维(b)与实施例1(c)、3(d) 包覆黄腐酚的纳米纤维膜的红外光谱图。从红外图谱中可以看到，实例1(c)和3(d) 不但在1756 cm-1和1188 cm-1均出现了PLGA的C=O和C-O特征吸收峰，而且实例1(c)和3(d)在1600-1450 cm-1还呈现出黄腐酚中苯环的特征峰，并且没有出现新的吸收峰和峰位移，说明黄腐酚、HA-g-PLLA和PLGA物理混合在一起。
图3为纯PLGA纤维(a) 和实施例1(b)、2(c)、3(d) 与4(e)包覆黄腐酚的纳米纤维的场发射扫描电镜图。纯PLGA与实例1（PLGA/黄腐酚）纤维表面光滑，直径均匀；加入HA-g-PLLA后纤维（实例2、3、4）直径明显增加，并且表面变得粗糙。
图4为纯PLGA纤维膜(a)和实施例1(b)、2(c)、3(d) 与4(e)包覆黄腐酚的纳米纤维膜的水接触角变化图。由图可见，与纯PLGA纤维膜相比，实例1（PLGA/黄腐酚）纤维膜的亲水性角随时间延长迅速减小，说明亲水性有了显著提高。然而加入HA-g-PLLA后纤维膜（实例2、3和4）的亲水角增到115°以上，并且在120s只有微小变化，三组份纤维膜呈现出更强的疏水性。
图5为实施例1(c)、2(a)、3(b)和4(d)包覆黄腐酚的纳米纤维膜的体外释放曲线。由图可见，随着时间的延长，各种载药纤维膜释放黄腐酚的量逐渐增加，在168h，实例1、2、3和4的累积释放率分别为32.45%，20.06%，26.43%和36.54%。对于三组份纤维来说（实例2，3，4），随着黄腐酚含量的增加释放速度逐渐加快。此外，当黄腐酚含量相同时，实例1释放黄腐酚的速率快于实例3。
具体实施方式
下面给出实施例以对本发明进行具体描述，但值得指出的是以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的技术熟练人员根据上述本发明内容对本发明做出的一些非本质的改进和调整仍属于本发明的保护范围。
实施例1：
(1) 纺丝液的配制：称取15 mg黄腐酚溶于3 g三氯甲烷/N,N-二甲基甲酰胺混合溶剂中；称取135 mg PLGA溶于上述溶液，最后加入0.5 wt% TEBAC，室温下磁力搅拌12 h，得到透明、均匀的纺丝溶液。
（2）纤维膜制备：室温下，纺丝溶液装入注射器，并将其固定在微量注射泵上；静电发生器的正极接于注射器前端的金属针头，接收装置（铝箔）连接负极；调节针头与接收装置的距离为20 cm；启动微量注射泵，流速设为12 μL/min，电源电压为7.7 kV，获得纤维膜在真空烘箱中25 ℃，干燥24 h。
实施例2：
（1）纺丝液的配制：称取7.5 mg HA-g-PLLA，置于3 g三氯甲烷/N,N-二甲基甲酰胺混合溶剂中，超声分散30 min，接着加入7.5 mg黄腐酚；称取135 mg PLGA溶于上述溶液，最后加入0.5 wt% TEBAC，室温下磁力搅拌12 h，得到透明、均匀的纺丝溶液。
（2）纤维膜制备：室温下，纺丝溶液装入注射器，并将其固定在微量注射泵上；静电发生器的正极接于注射器前端的金属针头，接收装置（铝箔）连接负极；调节针头与接收装置的距离为15 cm；启动微量注射泵，流速设为12 μL/min，电源电压为7.7 kV，获得纤维膜在真空烘箱中25℃，干燥24 h。
实施例3：
（1）纺丝液的配制：称取7.5 mg HA-g-PLLA，置于3 g三氯甲烷/N,N-二甲基甲酰胺混合溶剂中，超声分散30 min，接着加入15 mg黄腐酚；称取127.5 mg PLGA溶于上述溶液，最后加入0.5 wt% TEBAC，室温下磁力搅拌12 h，得到透明、均匀的纺丝溶液。
（2）纤维膜制备：室温下，纺丝溶液装入注射器，并将其固定在微量注射泵上；静电发生器的正极接于注射器前端的金属针头，接收装置（铝箔）连接负极；调节针头与接收装置的距离为15 cm；启动微量注射泵，流速设为12 μL/min，电源电压为7.7 kV，获得纤维膜在真空烘箱中25℃，干燥24 h。
实施例4：
（1）纺丝液的配制：称取7.5 mg纳米羟基磷灰石，置于3 g三氯甲烷/N,N-二甲基甲酰胺混合溶液中，加入0.5 wt% TEBAC，进行超声分散30 min，称取30 mg黄腐酚，112.5 mgPLGA溶于上述溶液，室温下磁力搅拌12 h，得到透明、均匀的纺丝溶液。
（2）纤维膜制备：室温下，纺丝溶液装入注射器，并将其固定在微量注射泵上；静电发生器的正极接于注射器前端的金属针头，接收装置（铝箔）连接负极；调节针头与接收装置的距离为15 cm；启动微量注射泵，流速设为12 μL/min，电源电压为7.7 kV，获得纤维膜在真空烘箱中25 ℃，干燥24 h。
最后应说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细的说明，本领域的普通技术人员应理解，对部分发明的技术方案进行修改或者同等替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (5)

1.一种包覆黄腐酚的纳米纤维膜，其特征在于以可生物降解的聚酯为基体，电纺丝制得聚酯/HA-g-PLLA/黄腐酚的复合纳米纤维膜材料，其中聚酯的含量为90～75wt％，HA-g-PLLA的含量为5wt％，黄腐酚的含量为5～20wt％，用合适的溶剂溶解，并搅拌得到均匀的纺丝液，利用静电纺丝装置制备包覆黄腐酚的纳米纤维膜。
2.如权利要求1所述的纳米纤维膜，所述的可生物降解的聚酯为聚ε-己内酯(PCL)、聚L-乳酸(PLLA)、聚乙交酯丙交酯(PLGA)中的一种或几种的混合物。
3.如权利要求1所述的纳米纤维膜，所述的溶剂为三氯甲烷、二氯甲烷、甲苯、二甲苯、三氯甲烷/N，N-二甲基甲酰胺混合溶剂、二氯甲烷/N，N-二甲基甲酰胺混合溶剂中的一种。
4.如权利要求1所述的纳米纤维膜，所述的静电纺丝装置的参数为纺丝电压5～20kV，两极间距离为10～20cm，纺丝液在喷丝口处的流速为0.3～1.5mL/h。
5.如权利要求1所述的纳米纤维膜，其应用于骨修复中。
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