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目的采用高效毛细管电泳法分离并测定瑞格列奈片中的对映异构体,探讨环糊精与对映异构体间的拆分机理。方法采用熔融石英毛细管柱(67 cm×75μm,有效长度60 cm),以20 mmol·L-1Tris(磷酸调p H3.9)-20 mmol·L-1羟丙基-β-环糊精(HP-β-CD)为运行缓冲液,分离电压20 k V,检测波长243 nm;优化手性选择剂的类型和浓度、缓冲液的组成和浓度、p H值、分离电压等条件。结果瑞格列奈5~50μg·m L-1与峰面积比值的线性关系良好,检测限为0.25μg·m L-1;S-(+)-瑞格列奈的平均回收率为97.15%,RSD=1.21%。结论所用方法具有良好的选择性、重复性和精密度,可用于瑞格列奈片中对映异构体的含量测定。
OBJECTIVE To separate and determine the enantiomers of repaglinide tablets by high performance capillary electrophoresis and investigate the mechanism of cyclodextrin and enantiomer separation. Methods The fused silica capillary column (67 cm × 75 μm and effective length of 60 cm) was used with 20 mmol·L-1 Tris (Phospho-p H3.9) -20 mmol·L-1 hydroxypropyl-β-cyclodextrin HP-β-CD) was used as the running buffer. The separation voltage was 20 kV and the detection wavelength was 243 nm. The optimal conditions of the type and concentration of chiral selector, the composition and concentration of buffer, p H value and separation voltage were optimized. Results The linear relationship between repaglinide 5 ~ 50μg · m L-1 and peak area ratio was good with a detection limit of 0.25μg · m L-1. The average recoveries of S - (+) - repaglinide were 97.15% , RSD = 1.21%. Conclusion The method used has good selectivity, repeatability and precision, which can be used for determination of enantiomers in repaglinide tablets.