分子印迹手性整体柱的制备及对非对映异构体的分离  

Preparation of Molecularly Imprinted Chiral Monolithic Column and Its Applications for Separation of Diastereomers

作　　者：黄晓冬[1] 邹汉法[1] 毛希琴[1] 罗权舟[1] 陈小明[1] 肖湘竹[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》2002年第5期436-438,共3页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目 (No 2 972 5512 ) .

摘　　要：采用原位分子印迹技术 ,单步制备了一种辛可宁印迹的手性整体柱。为了提高柱效和选择性 ,选择了相对低极性的甲苯 /十二醇复合致孔体系。在等度及梯度洗脱条件下 ,非对映异构体辛可宁与辛可尼丁被完全分离。等度洗脱中相对较宽的色谱峰可以在梯度洗脱中得到改善。同时考察了流动相中醋酸浓度、流速以及温度对分离的影响。由于柱中存在大的流通孔 ,大大降低了分离过程中的柱压降 ,从而使这种色谱柱能够在相对高的流速下使用。提高温度可以提高分离因子 ,在 60℃获得最大分离因子 5 40。A cinchonine imprinted chiral monolithic column was prepared for the separation of the diastereomers of cinchonine and cinchonidine by in situ molecular imprinting technique. This type of molecularly imprinted column can be prepared only by a single step procedure. In order to improve the selectivity and efficiency, a new in situ molecular imprinting polymerization system was introduced by adopting porogenic solvents of toluene and 1 dodecanol with relatively low polarity and appropriate ratios of polymerization mixture. Diastereomers of cinchonine and cinchonidine were fully separated both under isocratic and gradient elutions on the chiral monolithic column. The broad peak shown in isocratic elution could be improved in gradient elution. Effects of mobile phase composition, flow rate and temperature on retention and separation factor were investigated. Due to the large throughput pores in the chiral monolithic column, low backpressure was observed during the separation process and a separation factor of 3 18 was obtained at 1 0 mL/min. The increase of temperature could improve the separation factor and a maximum separation factor of 5 40 was obtained at 60 ℃.

关 键 词：手性整体柱 制备 分子印迹 原位聚合 手性分离 非对映异构体 色谱固定相 

分 类 号：O657.7[理学—分析化学] O658[理学—化学]