HPLC-MS/MS法鉴别中成药及保健品中添加的糖皮质激素类化学药物

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:SHIMADZU Shim-pack VP-ODS(250 mm×4.6 mm,5 μm)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20 mmol·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。

Objiective: To develop an HPLC-MS-MS method for identification of 14 kinds of corticosteroids illegally added to proprietary Chinese medicines and healthy foods. Method: The liquid chromatography-mass spectrometry method was used to detect the sample extracted with methanol.The HPLC chromatographic determinations were using SHIMADZU Shim-pack VP-ODS(250 mm×4.6 mm,5 μm) column,The 14 corticosteroids were designed into 2 groups.The mobile phase were grading of 20 mmol·L^-1 ammonium acetate solution (containing 0.1% formic acid,v/v) and acetonitrile.The mass spectrometer condition were as follows:the ionition mode was ESI⁺,the mode was mass scan and daughter scan,comparing 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 acetate and triamcinolone acetonide acetate was detected in 7 samples. Conclution: The developed method is accutate,sensitive and applicable to identify them.