LC-MS/MS法同时检测筋骨痛消胶囊中非法添加的醋酸泼尼松、双氯芬酸及布洛芬

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。

Simultaneous Determination of Prednisone Acetate, Diclofenac and Buprofen Illegally Added into Jingu Tongxiao Capsules by LC-MS/MS

To establish a detection method for prednisone acetate, diclofenac and buprofen illegally added into Jingu Tongxiao capsules by LC-MS/MS. Method： The detection was performed on a SHIMADZU shim-pack VP-ODS column （250 mm × 4. 6 mm ,5 μm） with the mobile phase of 0.02 mol· L^-1 ammonium acetate-0. 1% HAe solution and acetonitrile （53：47） at a flow rate of 1.0 ml.min^-1. The nebulizer pressure was 38psi and the dry temperature was 350℃. The scanning range was 50-500 m/z. Result： Chromatographic and mass spectra peak of the samples coincided with the reference prednisone acetate, diclofenac and buprofen, respec- tively. Conclusion： The method is exclusive, sensitive and credible, and it can be used to distinguish prednisone acetate, dielofenac and buprofen in Jingu Tongxiao capsules.