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

作　　者：黄晓冬[1] 孔亮[1] 厉欣[1] 陈学国[1] 郭宝川[1] 邹汉法[1] 

机构地区：[1]中国科学院大连化学物理研究所国家色谱研究分析中心,辽宁大连116011

出　　处：《色谱》2003年第3期195-198,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(29725512).

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。A cinchonine imprinted monolithic polymer was directly prepared in a capillary column by insitu 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 flowthrough pores were found in the optimized monolithic rod by scanning electron microscopy. Diastereomers of cinchonine and cinchonidine were separated in pressureassisted 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.

关 键 词：分子印迹 整体柱 毛细管电色谱 手性分离 非对映异构体 色谱柱 制备 抗疟药物 辛可宁 辛可尼丁 

分 类 号：O658[理学—分析化学] R978.3[理学—化学]