毛细管区带电泳测定唑来膦酸及其制剂的含量

Determination of zoledronic acid and its preparations by capillary zone electrophoresis

目的:建立简便、快速分析唑来膦酸及与其有关物质的毛细管区带电泳方法。方法:采用非涂渍石英毛细管(50cm×50 μm)为分离通道,3 mmol·L^(-1)磷酸盐缓冲液(pH 7.9)为运行缓冲体系;工作电压25 kV;进样电压2 kV,进样时间5 s;紫外检测波长为210nm。结果:唑来膦酸在31.2～998μg·mL^(-1)的范围内线性关系良好(r=0.9997);注射用唑来膦酸的平均回收率(n=9)为100.2%,RSD 为1.1%;唑来膦酸注射剂的平均回收率(n=9)为100.7%,RSD 为1.0%;最低检测限为10.4μg·mL^(-1),该条件下唑来膦酸与其有关物质分离良好。结论:本方法简便、快速、灵敏,为唑来膦酸生产合成中的质量控制提供了一种新的可靠的分析手段。

Objective：To estebalish a simple and rapid capillary zone electrophoresis method for the analysis of zoledronic acid and its related substance. Methods ：An uncoated fused - silica capillary column of 50 cm×50 μm was used. The method was developed by utilizing a eleetrokinetic injection（2 kV,5 s） , a running voltage of 25 kV and a 3 mmol·L^-1 phosphate electrolyte solution at pH 7.9. The detection wavelength was 210 nm. Results：The calibration curve was linear in the range of 31.2 -998μg ·mL^-3（r =0. 9997） ,the average recovery of zoledronie acid for injection was 100.2% with RSD of 1.1% ;for zoledronic acid injection the average recovery was 100.7% with RSD of 1.0% ;the LOD was 10. 4μg·mL^-1 ,the active ingredient - zoledronic acid was successfully separated from its related substance. Conclusion： The method is simple, rapid and accurate ; it provides a new reliable means for the quality control of zoledronic acid.