摘要
目的:研究尼群地平对映体在ChiralcelOJ柱上的拆分特性和规律。方法:采用高效液相色谱法,色谱柱为纤维素键合OJ手性柱(250mm×4.6mm,10μm),流动相为正己烷-无水乙醇,检测波长为236nm,流速为0.5mL/min。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:尼群地平R-对映体的lgI值均高于S-对映体,置换剂无水乙醇对对映体拆分有不同的影响;三乙胺浓度增加,对映体的保留和拆分效率均减小;随柱温从4~40℃改变,对映体间的分离度出现极值。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ChiralcelOJ柱的拆分能力和对映体空间效应,三乙胺使拆分效率降低,适当的柱温可以改善和提高拆分效果。
Objective: To study the cnantioselective characteristics and laws of Nitrendipine enantiomers on Chiralcel OJ column. Methods: The experiments were performed under the HPLC conditions as following: the Chiralcel OJ column (250 mm ×4.6mm,10μm) as analytical column, mobile phase consisting of a mixture of n - hexane/ethanol, the detection wavelength at 236 nm and a flow rate of 0. 5 mL/min. The effects of stationary phase and ethanol concentration in mobile phase on the enantiomer resolution were investigated by the stoichiometric displacement model for retention (SDM- R). So did as that of triethylamine concentration and the column temperature as well. Results: The lgl values of R-enantiomer of Nitrendipine was higher than that of S- enantiomer. The ethanol in mobile phase would differently affect the resolution between enantiomers for Nitrendipine. The capacity factor (k') and the resolution of the enantiomers would decrease with increasing the triethylamine concentration in mobile phase. The resolution appeared a maximum value with column temperature varied from 4℃ to 40℃. Conclusion: The lgl and Z values of SDM- R could be employed to characterize the resolution efficacy of Chiralcel OJ column and the space effect of enanliomcrs interacted with the stationary phase. Adding triethylamine in mobile phase would decrease the resolution efficacy and changing column temperature could promote the enantiomer resolution.
出处
《中国药业》
CAS
2006年第3期23-24,共2页
China Pharmaceuticals
基金
国家自然科学基金资助项目
项目编号:30171080。