β-受体阻滞剂对映体在Chiralcel~OD手性柱上的拆分特性

The separation of β-adrenoceptor antagonist enantiomers on Chiralcel~ OD column

目的 研究 β 受体阻滞剂对映体在Chiralcel○R手性柱上的拆分特性和规律。方法 色谱柱为Chiralcel○ROD手性柱 (2 5 0mm× 4 .6mm ,10 μm) ,流动相为正己烷 异丙醇 三乙胺 ,荧光检测激发波长 λex2 75nm ,发射波长λem310nm。用溶质计量置换保留模型考察固定相和流动相中置换剂强度对拆分的影响 ,同时考察三乙胺及温度对保留与拆分的影响。结果 考察了 5种 β 受体阻滞剂 ,其中 3种 β 受体阻滞剂对映体在选定色谱条件下均得到了基线分离 ,其R 对映体的lgI值均高于S 对映体 ,置换剂异丙醇对各对映体拆分有不同的影响 ;三乙胺浓度的增大 ,各对映体的保留减小 ,而分离度增加 ;柱温升高 ,各对映体的保留及分离度均降低。结论 溶质计量置换保留模型的计量置换参数lgI和Z值 ,可以分别表征ChiralcelOD柱的拆分能力和各对映体空间效应 ;增加三乙胺浓度可提高拆分效率 。

Objective To study the enantioselective characteristics and laws of β-adrenoceptor antagonist isomers on Chiralcel ○R OD column. Methods The experiments were performed under the following HPLC conditions: a Chiralcel OD column (250 mm×4.6 mm, 10 μm) as analytical column, a mixture of n-hexane/2-propanol/ triethylamine as the mobile phase, the fluorescence detection wavelengths at 275 nm (λ ex) and 310 nm (λ em), and the flow rate at 0.5 mL·min -1. The effect of interaction between stationary phase and 2-propanol or triethylamine concentration in mobile phase on the enantiomer resolution were investigated by the stoichiometric displacement model for retention. Results The lgI values of R-enantiomers of 3 out of 5 β-adrenoceptor antagonist were higher than those of S-enantiomers. The 2-propanol in mobile phase would differently affect the resolution between enantiomers for each β-adrenoceptor. With the increase of triethylamine concentration in mobile phase, the capacity factor (k′) of the enantiomers decreased but the resolution increased. Conclusion The lgI and Z values of SDM-R could be employed to characterize the resolution efficiency of Chiralcel OD column and the specific effect of enantiomers interacted with the stationary phase. Adding triethylamine in mobile phase will increase the resolution efficacy and changing column temperature can promote enantiomer resolution.