高效毛细管电泳法测定瑞格列奈片中的对映异构体

Determination of Repaglinide enantiomers by high performance capillary electrophoresis

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 establish an HPCE method for the chiral separation and determination of Repaglinide enantiomers,and to discuss the seperation mechanism of CD and enantiomers. METHODS An uncoated fused sillica capillary column（ 60 cm × 50μm,effective length was 60 cm） was used with running buffer of 20 mmol·L^-1Tris（ hydroxymethyl） aminomethane（ adjusted to p H3. 9 with phosphoric acid）-20 mmol·L^-12-hydroxypropyl-β-cyclodextrin at the applied voltage of 20 k V and the detection wavelength of 243 nm. Under the optimized conditions,a base-line separation of enantiomers of Repaglinide were achieved. Several parameters were optimized for a satisfactory enantioresolution,including the composition of the running buffer,the types and concentration of chiral selectors,the p H value,separation voltage,injection time and capillary ＇s inside diameter and detection wavelength.RESULTS The calibration curve for Repaglinide was linear in the concentration range of 5-50 μg·m L-1with the limits of detection of 0. 25 μg·m L^-1. The average recovery was 97. 15%,and the RSD was 1. 21%. CONCLUSION The method has good selectivity,repeatability and accuracy. It can be applied to investigate the enantiomeric purity of Repaglinide.