高效液相色谱手性流动相添加剂分离西孟坦对映体  

High Performance Liquid Chromatographic Separation of Simendan Enantiomer Using Chiral Mobile Phase Additive

作　　者：张丹丹[1] 郭兴杰[1] 袁波[1] 李发美[1] 

机构地区：[1]沈阳药科大学药学院分析化学教研室,沈阳110016

出　　处：《分析化学》2004年第2期229-231,共3页Chinese Journal of Analytical Chemistry

摘　　要：以 β 环糊精作为手性流动相添加剂 ,研究了DL 西孟坦在反相HPLC系统中的拆分。考察了缓冲盐的浓度、pH、β 环糊精的浓度、流动相中甲醇的比例、流动相流速和温度对手性分离的影响 ,建立了 β 环糊精动态手性固定相法分离西孟坦对映体的方法。色谱条件为 :ZirchromKromasilODS 1(5 μm ,15 0mm× 4 .6mm)色谱柱 ,流动相为 2 0mmol/L磷酸盐缓冲液 (pH 6 .0 )含 12mmol/Lβ 环糊精∶甲醇 (70∶30 ,V/V) ,流速为 0 .8mL/min ,温度为 17℃。DL 西孟坦对映体的保留时间分别为 2 2 .5和 2 4 .5min ,分离度为 1.5 7。The enantiomeric resolution of Simendan was studied by using reversed-phase high performance liquid chromatography with β-cyclodextrin (β-CD) as chiral mobile phase additive. The influences of the concentration of buffer solution and chiral mobile phase additive, pH, temperature and flow rate on the resolution were investigated. The chromatographic systems with a dynamically-generated stationary phase with β-cyclodextrin was proved to be an effective method for Simendan enantiomer separation. Zirchrom Kromasil ODS-1(5 μm,150 mm×4.6 mm i.d.) column was used. The optimized mobile phase was 20 mmol/L phosphate buffer (pH 6.0) containing 12 mmol/L β-cyclodextrin-methanol(70∶30, V/V) with the flow rate set at 0.8 mL/min and the temperature of 17℃. The retention time of L-Simendan and D-Simendan were 22.5 min and 24.5 min, a resolution of 1.57 was achieved.

关 键 词：DL-西孟坦 对映体 分离 高效液相色谱 手性流动相添加剂 Β-环糊精 心脏兴奋药 

分 类 号：O657.7[理学—分析化学]