西酞普兰对映体的手性色谱拆分及吸附平衡

摘要

The enantioseparation of citalopram enantiomers was investigated using high performance liquid chromatography to optimize chromatographic conditions. Chiral stationary phases ( CSPs) including derivatized polysaccharide CSPs, crosslinked diallyltartrinine amide CSPs and cyclodextrin-based CPSs were used as stationary phases. N-Hexane with a small amount of diethylamine (0. 1% , volume) modified with methanol, ethanol and 2-propanol were used as mobile phase. The influence on retention factor, enantioselectivity, resolution, theoretical plates and asymmetry factor were studied. The effect of temperature was also investigated on the most favorable CSP and mobile phase. Chiralpak AD-H (derivatized polysaccharide CSP) and 2-propanol were proved to be the most favorable CSP and modifier, and 5% (vol) of 2-propanol was the preferred concentration. It was found that among the temperature range of 293. 15-308. 15 K, higher temperature was favorable to the enantioseparation. The adsorption isotherms of citalopram enantiomers were determined by frontal analysis chromatography under the optimized chromatographic conditions. The isotherms showed convex shape and well fitted by the Langmuir adsorption isotherm model. This work provides the basic data for separation of citalopram on SMB.%以添加醇类和二乙胺的正己烷为流动相,考察了多糖类、酒石酸类和环糊精类手性固定相对西酞普兰外消旋体的拆分效果,优选合适的手性固定相、流动相和温度等色谱条件,在此基础上利用前沿色谱法测定了西酞普兰对映体的吸附等温线.优化的色谱操作条件为:Chiralpak ADH柱为固定相,正己烷:异丙醇:二乙胺(95∶5∶0.1,体积比)为流动相,柱温35℃.西酞普兰对映体的吸附等温线为优惠型,采用Langmuir方程拟合,效果较好.本研究为模拟移动床(SMB)制备西酞普兰对映体提供重要的基础数据.