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建立了一种高效液相色谱-串联质谱(HPLC-MS/MS)测定水产品中氢化可的松残留的检测方法。样品经乙酸乙酯和正己烷提取,用OasisHLB固相萃取柱净化,然后选用电喷雾离子源(ESI),在负离子、多反应监测方式(MRM)模式下进行定性,以外标法进行定量。方法的定量限为2.0ng/g,工作曲线的线性范围为2.0~200.0ng/mL。在添加浓度为2.0～10.0ng/g的范围内,氢化可的松的平均回收率范围为99.3%~106.0%之间,相对标准偏差在2.62%~7.71%之间。方法快速、准确、检出限低、实用性强、特异性好。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was developed for the determination of hydrocortisone residues in aquatic products. The sample was extracted with ethyl acetate and n-hexane, purified with OasisHLB solid phase extraction column, and then electrospray ionization (ESI) was selected for qualitative analysis in negative ion and multiple reaction monitoring (MRM) mode and quantified by external standard method. The limit of quantification was 2.0 ng / g and the linear range of the working curve was 2.0 ~ 200.0 ng / mL. The average recoveries of hydrocortisone ranged from 99.3% to 106.0% and the relative standard deviations (RSDs) ranged from 2.62% to 7.71% at the range of 2.0 ~ 10.0ng / g. The method is rapid, accurate, with low detection limit, good practicability and good specificity.