UPLC/MS/MS法检测抗风湿类制剂中添加醋酸泼尼松、醋酸地塞米松、双氯芬酸钠和布洛芬

UPLC/MS/MS determination of prednisone acetate,dexamethasone acetate,diclofenac sodium and ibuprofen mixed in antirheumatic traditional Chinese medicine

目的:建立快速、准确、灵敏的检测抗风湿类中药制剂中非法添加醋酸泼尼松、醋酸地塞米松、双氯芬酸钠和布洛芬的分析方法。方法:采用ACQUITYBEHC18色谱柱(2.1mm×50mm,1.7μm),0.02mol·L-1醋酸铵溶液(A)-乙腈(B)梯度洗脱,流速0.3mL·min-1,检测波长263nm;离子源为ESI源,正负离子同时检测,对中药制剂中非法添加醋酸泼尼松、醋酸地塞米松、双氯芬酸钠和布洛芬进行定性、定量检测。结果:受试制剂中检测到掺有醋酸泼尼松、双氯芬酸钠。结论:此方法灵敏准确,可作为抗风湿类中药制剂中非法添加醋酸泼尼松、醋酸地塞米松、双氯芬酸钠和布洛芬的有效检测方法。

Objective：To establish a quick,accurate,sensitive method for analysis of prednisone acetate,dexamethasone acetate,diclofenac sodium and ibuprofen mixed in antirheumatic traditional Chinese medicine by UPLC/MS/MS.Methods：The chromatographic conditions included ACQUITY BEH C18 analysis column（2.1 mm×50 mm,1.7 μm）,mobile phase of 0.02 mol·L-1 ammonium acetate（A）and acetonitrile（B）with gradient elution,flow rate of 0.3 mL·min-1,the detection wavelength was set at 263 nm.Electrospay ionization（ESI）source was applied and operated in the positive and negative ion mode.Prednisone acetate,dexamethasone acetate,diclofenac sodium and ibuprofen mixed in traditional Chinese medicinal were identified.Results：Both prednisone acetate and diclofenac sodium were found in formulationgs.Conclusion：The method is sensitive and accurate,and can be used to detect the prednisone acetate,dexamethasone acetate,diclofenac sodium and ibuprofen mixed in antirheumatic traditional Chinese medicine.