分子印迹技术靶向制备三七素和天麻素

发布时间：2018-07-28 15:12

【摘要】：三七素是传统名贵中草药三七(Panax notoginseng(Burk.)F.H.Chen)中的止血成分,其止血活性要优于止血环酸,是一种良好的止血剂。天麻素是天麻(Gastrodia elata Blume)中的主要活性成分,具有镇痛、镇静、催眠、抗惊厥、保护神经系统和延缓衰老等生理作用。三七素和天麻素都是水溶性化合物,属于高极性、小分子化合物,分离纯化十分困难。三七和天麻成分复杂多样,传统分离方法效率低下。因此,建立一种高效分离制备方法实现三七素和天麻素的分离纯化十分必要。本论文充分利用分子印迹聚合物具有特异识别性的特点,通过分子印迹技术制备了对三七素和天麻素具有高度选择识别性和高吸附容量的聚合物,将聚合物用作固相萃取吸附填料,定向分离制备药材三七和天麻中的三七素和天麻素。1.表面分子印迹聚合物靶向制备三七素以硅胶为载体,以丙烯酰胺(AM)为功能单体、二甲基丙烯酸乙二醇酯为交联剂(EGDMA)、乙腈为致孔剂,优化制备了假模版表面分子印迹聚合物(surface dummy molecularly imprinted polymers,SDMIPs)。吸附实验证明以D-亮氨酰甘氨酸(LG)为模板分子制备的聚合物对三七素的吸附性能最好,最大吸附容量为0.185mmol/g,在15 min内即能达到吸附平衡。将聚合物用作固相萃取填料靶向分离三七素,得到三七素纯度高达98.7%,平均回收率为83.7%。实验证明表面分子印迹聚合物适合作为固相萃取填料从三七中分离富集三七素。2.亲水性分子印迹聚合物靶向制备天麻素在实验室前期工作的基础上,水解疏水性天麻素分子印迹聚合物表面酯基,制备亲水性天麻素分子印迹聚合物(hydrophilic molecularly imprinted polymers,H-MIPs)。红外光谱显示聚合物表面部分酯基水解形成羟基,亲水性测试结果证明聚合物具有良好的亲水性。吸附实验结果显示与疏水性分子印迹聚合物相比,亲水性分子印迹聚合物对天麻素具有更快的吸附速率和更高的吸附量。将该聚合物装填SPE柱分离富集天麻素,得到天麻素纯度高达98.8%,平均回收率为87.5%。实验证明H-MIPs更适合作为固相萃取柱填料从天麻中靶向制备天麻素。
[Abstract]:The 37 element is the traditional Chinese herbal medicine 37 (Panax notoginseng (Burk.) F.H.Chen) hemostasis composition, its hemostatic activity is better than the hemostatic acid, is a good hemostatic agent. Gastrodin is the main active component of Gastrodia elata (Gastrodia elata Blume), with analgesic, sedative, hypnotic, anticonvulsant, protection of the nervous system and postponing senescence. 37 elements and gastrodin are water-soluble compounds, which are highly polar, small molecular compounds, and are very difficult to separate and purify. 37 and the composition of Gastrodia elata are complex and diverse, and the traditional separation method is inefficient. Therefore, it is necessary to establish a high efficient separation method for the separation and purification of 37 elements and gastrodin. Using molecularly imprinted polymer with specific recognition characteristics, polymers with highly selective recognition and high adsorption capacity for 37 elements and gastrodin are prepared by molecular imprinting technology. The polymer is used as solid phase extraction adsorption filler, and 37 elements in medicinal herbs and gastrodin.1. surface molecular printing are prepared by directional separation. The trace polymer was targeted to prepare 37 prime samples with silica gel as carrier, acrylamide (AM) as functional monomer, two ethylene glycol methacrylate as cross linker (EGDMA) and acetonitrile as a pore agent. The pseudo template surface molecularly imprinted polymer (surface dummy molecularly imprinted polymers, SDMIPs) was prepared. The adsorption experiment proved to be a D- leucyl glycoline. The polymer prepared by acid (LG) for template molecule has the best adsorption properties for 37 elements, the maximum adsorption capacity is 0.185mmol/g, and the adsorption equilibrium can be reached within 15 min. The polymer is used as the solid phase extraction filler target separation 37, the purity of 37 elements is as high as 98.7%, and the average recovery rate is 83.7%. experiment to prove the surface molecularly imprinted polymer The hydrophilic gastrodin molecularly imprinted polymer (hydrophilic molecularly imprinted polymer) was prepared and prepared on the basis of the preparation of.2. hydrophilic molecularly imprinted polymer (hydrophilic molecularly imprinted polymer) as solid phase extraction filler. S, H-MIPs). The IR spectra showed that the hydroxyl groups were formed by hydrolysis of the polymer surface on the surface of the polymer. The hydrophilic test results showed that the polymer had good hydrophilic properties. The concentration of gastrodin was separated and enriched by SPE column. The purity of gastrodin was up to 98.8%. The average recovery rate of 87.5%. proved that H-MIPs was more suitable for the preparation of gastrodin from Gastrodia elata as solid phase extraction column.
【学位授予单位】：山东农业大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：TQ461;O631.3

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