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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 establish the identification method of illegally added diclofenac in Wu snut Puerariae by LC-MS / MS. METHODS: The mobile phase consisted of Shimadzu Shim-pack VP-ODS (250 mm × 4.6 mm, 5 μm), 0.02 mol·L-1 ammonium acetate-0.1% acetic acid in water and acetonitrile (55:45) at a flow rate of 1.0 mL. min-1, detection wavelength was 280 nm; Agilent6310 ion trap mass spectrometer, electrospray ionization source (ESI), atomizing gas pressure 27.6 kPa, drying temperature 350 ℃, flow rate 9 mL.min- 150 ~ 500. Results: In HPLC, mass spectrometry, the sample showed peaks consistent with diclofenac composition, mass spectrum peak. Conclusion: The method is simple and feasible, the results are accurate and reliable, and can be used for the qualitative identification of diclofenac added in the Hu Shek Kudzu capsule.