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原位分子印迹毛细管电色谱柱的制备及其对非对映异构体的分离
Preparation of Molecularly Imprinted Monolithic Capillary Column for Separation of Diastereomers of Cinchona Alkaloids by Pressure-Assisted Capillary Electrochromatography
【摘要】 采用原位聚合的方法直接在毛细管柱中合成出辛可宁印迹聚合物。该聚合物与毛细管内壁共价结合连为一体形成整体式毛细管柱,扫描电镜显示其具有大的流通孔结构。采用压力辅助毛细管电色谱模式拆分了非对映异构体抗疟药物辛可宁和辛可尼丁,柱效远高于其在高效液相色谱分离中的柱效。考察了电压、外压、温度、流动相表观pH值和乙腈含量对分离结果的影响。通过对上述条件的优化,可以在2min内完成辛可宁和辛可尼丁的快速分离。
【Abstract】 A cinchonine imprinted monolithic polymer was directly prepared in a capillary column by insitu polymerization, and the polymer was covalently linked to the activated inner surface of the capillary tube, which sustained the polymer not to move in operation. The permeability of the monolithic polymer can be simply controlled by changing the polymerization temperature. Large flowthrough pores were found in the optimized monolithic rod by scanning electron microscopy. Diastereomers of cinchonine and cinchonidine were separated in pressureassisted capillary electrochromatography mode due to low electroosmotic flow in operation, and the resulted separation efficiency was much higher than that obtained in high performance liquid chromatography. The effects of applied voltage, pressure, temperature, apparent pH and the contents of acetonitrile in mobile phase on retention time and resolution were investigated. As the retention times of cinchonine and cinchonidine were decreased with the increase of voltage, applied pressure and temperature, a rapid separation of cinchonine and cinchonidine can be obtained within 2 min under optimized conditions.
【Key words】 molecular imprinting; monolithic column; capillary electrochromatography; chiral separation; diastereomers;
- 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2003年03期
- 【分类号】O658
- 【被引频次】85
- 【下载频次】607