超临界流体色谱技术在西替利嗪对映体拆分中的应用

Enantiomeric Separation of Cetirizine by Supercritical Fluid Chromatography

目的:采用超临界流体色谱技术,以超高效合相色谱系统建立一种西替利嗪对映体的拆分方法。方法:利用超高效合相色谱系统,采用ACQUITY UPC2Trefoil手性色谱柱,以超临界二氧化碳为流动相中主要组分,对西替利嗪的左旋体和右旋体进行拆分,检测波长为228 nm。以左西替利嗪的保留时间、分离度、对称因子和理论塔板数为指标,考察手性柱的种类、改性剂与添加剂的种类和比例、柱温、背压、流速等对手性分离的影响。结果:优选色谱条件为使用ACQUITY UPC2Trefoil CEL1柱(2.1 mm×50 mm,2.5μm),改性剂为甲醇-乙腈(5∶6)在流动相中的占比为13%、添加剂为二乙胺在改性剂中的占比为0.8%(v/v),柱温45℃,背压1 600 psi,流速为0.6 ml·min^(-1)。此时西替利嗪对映体的分离度为2.107,对称因子为1.328,理论塔板数为2 409,分离效果好。结论:采用超临界流体色谱技术,以超高效合相色谱系统能够完全分离西替利嗪对映体,是一种环保、简便、高效的分析方法。

Objective: To establish a method to separate cetirizine enantiomers by ultra-performance convergence chromatography( UPC2) using supercritical fluid chromatography. Methods: Using UPC2,cetirizine levo isomer and dextro isomer were separated on ACQUITY UPC2 Trefoil chiral columns with supercritical carbon dioxide as the mobile phase,and the detection wavelength was 228 nm. With the retention time,resolution,symmetry factor and theoretical plate number of levocetirizine as the indices,the effects of chiral column types,types and proportions of modifiers and additives,column temperature,backpressure and flow rate on the chiral separation were investigated. Results: The selected chromatographic conditions were using an ACQUITY UPC2 Trefoil CEL1 column( 2. 1 mm × 50 mm,2. 5 μm),the modifier was methanol-acetonitrile( 5 ∶ 6) and the proportion in the mobile phase was 13%,the additive was diethylamine and the proportion in the modifier was 0. 8%( v/v),the column temperature was 45 ℃,the backpressure was 1 600 psi,and the flow rate was 0. 6 ml · min^-1. Under the optimized conditions,the resolution of cetirizine enantiomers was 2. 107,the symmetry factor was 1. 328 and the theoretical plate number was 2 409. Under the above conditions,the separating effect was good. Conclusion: Using supercritical fluid chromatography,cetirizine enantiomers can be completely separated by ultra-performance convergence chromatography,which is an environmental friendly,simple and efficient analytical method.