LC-MS/MS法对乌蛇葛根胶囊中非法添加双氯芬酸的检查

LC-MS/MS detection of diclofenac in Wushegegen capsules

目的:采用LC-MS/MS联用技术,建立乌蛇葛根胶囊中非法添加双氯芬酸的鉴别方法。方法:色谱柱为Shimadzu Shim-pack VP-ODS(250 mm×4.6 mm,5μm),0.02 mol.L-1醋酸铵-0.1%醋酸水溶液及乙腈(55∶45)为流动相,流速1.0 mL.min-1,检测波长为280 nm;Agilent6310离子阱质谱仪,电喷雾离子源(ESI),雾化气压力27.6 kPa,干燥气温度350℃,流速9 mL.min-1,扫描范围m/z 150～500。结果:在高效液相色谱、质谱中,样品出现与双氯芬酸成分一致的色谱峰、质谱峰。结论:本方法简单可行,结果准确可靠,可用于乌蛇葛根胶囊中添加双氯芬酸成分的定性鉴别。

Objective：To develop a detection method for diclofenac illegally added in Wushegegen capsules by LC-MS/MS.Methods：The detection was performed on a Shimadzu Shim-pack VP-ODS（250 mm×4.6 mm,5 μm） with a mobile phase of 0.02 mol·L-1 ammonium acetate-0.1% acetic acid solution and acetonitrile（55∶45） at a flow rate of 1.0 mL·min-1;The detection wavelength was 280 nm.The nebulizer pressure was 27.6 kPa and the dry temperature was 350 ℃;The scan range was m/z 150-500.Results：Chromatographic and mass peaks coinciding with that of diclofenac reference substance were found in the sample.Conclusion：The method is simple,sensitive and accurate,and can be used to identify diclofenac in Wushegegen capsules.