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目的:采用LC-MS/MS联用技术建立检测筋骨痛消胶囊中非法添加醋酸泼尼松、双氯芬酸及布洛芬的方法。方法:色谱柱为SHIMADZU shim-pack VP-ODS(250mm×4.6mm,5μm),0.02mol·L~(-1)醋酸铵0.1%醋酸水溶液:乙腈(53:47)为流动相,流速1.0ml·min~(-1);Agilent6310离子阱质谱仪,电喷雾离子源(ESI),雾化气压力38psi,干燥气温度350℃,流速9ml·min~(-1),扫描范围50～500m/z。结果:在高效液相色谱、质谱中,样品出现与醋酸泼尼松、双氯芬酸及布洛芬成分一致的色谱峰、质谱峰。结论:本方法选择性强,灵敏度高,可用于筋骨痛消胶囊中非法添加醋酸泼尼松、双氯芬酸及布洛芬的定性鉴别。
OBJECTIVE: To establish a method for the detection of the illegal addition of prednisone acetate, diclofenac and ibuprofen in Gushu Tongxiao capsule by LC-MS / MS. Methods: The mobile phase was SHIMADZU shim-pack VP-ODS (250mm × 4.6mm, 5μm), 0.02mol·L -1 ammonium acetate 0.1% acetic acid aqueous solution and acetonitrile · Min ~ (-1); Agilent6310 ion trap mass spectrometer, electrospray ionization source (ESI), atomization gas pressure 38psi, drying temperature 350 ℃, flow rate 9ml · min -1, scanning range 50 ~ 500m / z. Results: In HPLC and mass spectrometry, the samples showed the same peaks and peaks as the components of prednisone acetate, diclofenac and ibuprofen. Conclusion: The method is selective and sensitive. It can be used for the qualitative identification of prednisone acetate, diclofenac and ibuprofen illegally added to Gutou Tongxiao Capsule.