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目的:建立HPLC-MS/MS法检测中成药及保健品中可能非法添加的泼尼松、地塞米松、曲安萘德、醋酸泼尼松龙、醋酸氢化可的松、醋酸泼尼松、醋酸可的松、醋酸地塞米松、醋酸曲安萘德、泼尼松龙、氢化可的松、倍他米松、醋酸氟轻松、丙酸倍氯米松等14种糖皮质激素类化学药物。方法:样品经甲醇提取,采用液相色谱-质谱联用法测定。色谱条件:SHIMADZUShim-packVP-ODS(250mm×4.6mm,5μm)色谱柱,14种糖皮质激素类化合物分为两个液相系统,分别以20mmol.L-1醋酸铵(含0.1%甲酸,v/v)-乙腈进行梯度洗脱,质谱条件:电喷雾离子化正离子检测方式(ESI+),全扫描一级质谱、选择离子二级扫描质谱检测方式,通过与标准谱库中保留时间和多级质谱图的双重对比,对样品中非法添加的糖皮质激素类化学药物进行定性鉴别。结果:在50批供试品中,检测到有7种样品中含有醋酸泼尼松和醋酸曲安萘德。结论:本测定方法准确、灵敏度高,可满足定性研究的要求。
Objective: To establish a HPLC-MS / MS method for the determination of prednisone, dexamethasone, triamcinolone acetonide, prednisolone acetate, hydrocortisone acetate, prednisone acetate, Cortisone acetate, dexamethasone acetate, triamcinolone acetonide, prednisolone, hydrocortisone, betamethasone, fluocinolone acetonide, beclomethasone propionate and other 14 glucocorticoid chemicals. Methods: The samples were extracted by methanol and determined by liquid chromatography-mass spectrometry. Chromatographic conditions: SHIMADZUShim-packVP-ODS (250mm × 4.6mm, 5μm) column, 14 glucocorticoid compounds were divided into two liquid phase systems, respectively, with 20mmol.L-1 ammonium acetate / v) -acetonitrile. The conditions of mass spectrometry were as follows: positive ion electrospray ionization (ESI +), full scan one mass spectrometry, selective ion two-scan mass spectrometry detection method, Level spectrum of the double comparison, illegally added to the sample of glucocorticoid chemicals qualitative identification. Results: Of the 50 batches tested, 7 samples were found to contain prednisone acetate and triamcinolone acetonide. Conclusion: The method is accurate and sensitive, which can meet the requirements of qualitative research.