HPLC-ESI-MS法同时检测抗风湿中成药制剂中非法添加肾上腺糖皮质激素类化学药品泼尼松等6种成分研究

HPLC-ESI-MS Identification of Six Kinds of Corticosteroids Prednisone,etc. Chemicals Illegally Added to Chinese Medicines

目的:建立HPLC-ESI-MS法测定中成药制剂抗风湿药中有可能非法添加地塞米松、醋酸地塞米松、醋酸氢化泼尼松、醋酸氟氢松、氢化可的松、醋酸泼尼松等6种常用肾上腺糖皮质激素类化学药成分。方法:采用液质联用技术测定。色谱条件:Thermo ODS HYPERSIL(2.1μm×150mm,5μm)色谱柱,以乙腈-水梯度洗脱,检测波长240nm,流速0.2mL·min-1,进样量20μL;质谱条件:离子源为电喷雾离子化源(ESI源),源喷雾电压4500v,加热毛细管温度270℃,鞘气(N2)10,辅气(N2)20,正离子方式检测,扫描方式为一级全扫描、二级全扫描质谱,扫描范围150～550,扫描时间为0.129s。结果:根据检测到的化合物的色谱保留时间及一级、二级质谱信息,并与对照品比较,可作为分析检测中药制剂中非法添加上述6种肾上腺糖皮质激素类化学药的有效手段。结论:该检测方法选择性强,灵敏度高,定性准确。

Objectlve：To establish a HPLC -ESI -MS method for identification of 6 kinds of conu, non corticostemids ille- gally added to Chinese medicines. Methods：This analysis was performed by a LC -MS/MS system. The HPLC chromatographic determinations were using Thermo ODS HYPERSIL（2. 1μm×150mm,5μm）column, Gadient elution is done with water and ace- tonitrile. The flow rate was 0. 2ml·min -1 with detection wavelength at 240nm. The mass spectrometer condition were as follow： the ionltion mode was ESI ＋ ,the mode was mass scan ang daughter scan, compar/ng with retention time and spectra of references in library set up by ourselves, and the target compounds in sample were screened and identified. Results：Prednisone etc. was detected in samples. Conclusion ：The developed method is accurate, sensitive and applicable to identify them.