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目的:建立同时测定蛇酒中醋酸泼尼松、醋酸氢化可的松、醋酸地塞米松、布地奈德和甲泼尼龙的快速高分离液相色谱-电喷雾质谱联用方法。方法:采用Agilent Poroshell 120 EC-C18色谱柱(100mm×3mm,2.7μm),乙腈(含0.1%甲酸)-0.1%甲酸水溶液为流动相进行梯度洗脱,流速0.3m L/min;采用电喷雾离子源,以正离子、多反应监测扫描模式对蛇酒中的5种糖皮质激素进行定性定量检测,并对其裂解方式进行解析。结果:醋酸泼尼松、醋酸氢化可的松、醋酸地塞米松、布地奈德和甲泼尼龙线性关系良好,R2均>0.99,8种蛇酒中检测到糖皮质激素。结论:本研究建立的快速高分离液相色谱-电喷雾质谱联用法方便快捷、灵敏度好、准确度高,适用于蛇酒中非法添加成分的定性定量检测。
OBJECTIVE: To establish a rapid and high performance liquid chromatography-electrospray ionization mass spectrometry method for simultaneous determination of prednisone acetate, hydrocortisone acetate, dexamethasone acetate, budesonide and methylprednisolone in snake wine. Methods: The gradient elution was carried out on an Agilent Poroshell 120 EC-C18 column (100 mm × 3 mm, 2.7 μm) with acetonitrile (containing 0.1% formic acid) and 0.1% formic acid as mobile phase at a flow rate of 0.3 mL / min. Ion source, positive ions, multiple reaction monitoring scan mode of snake wine in five kinds of glucocorticoid qualitative and quantitative detection, and its cleavage method was analyzed. RESULTS: Prednisone acetate, hydrocortisone acetate, dexamethasone acetate, budesonide and methylprednisolone had good linear relationships with R2> 0.99 and glucocorticoids were detected in 8 snake wines. Conclusion: The rapid, high performance liquid chromatography coupled with electrospray ionization mass spectrometry established in this study is convenient, rapid, sensitive and accurate. It is suitable for qualitative and quantitative detection of illegally added components in snake wine.