快速滤过型净化结合液相色谱-质谱联用法测定海产品中19种磺胺类药物残留

建立了快速滤过型净化(m-PFC,multi-plug filtration cleanup)结合液相色谱-质谱联用技术同时检测海产品中19种磺胺类药物的分析方法。样品加水浸润后经过甲酸乙腈提取,QuEChERS盐包分层,取上层提取液经m-PFC柱净化,液相色谱-质谱联用测定,采用多反应监测模式(MRM)进行分析,基质外标法定量。结果表明,19种磺胺类药物在1～100μg/L的范围内线性关系良好,决定系数大于0.997,检出限为0.005～0.15μg/kg,定量限为0.01～0.41μg/kg。在10、20、100μg/kg三水平的平均添加回收率为70.0%～114.1%,相对标准偏差为0.5%～9.4%。该方法操作简便、快速,灵敏度高,重现性好,适用于海产品中多种磺胺类药物残留的检测。

Determination of 19 Sulfonamides Residues in Seafood by Multi-plug Filtration Cleanup Method Combined with Liquid Chromatography-Tandem Mass Spectrometry

A method was established for simultaneous detection of 19 sulfonamides in seafood by multi-plug filtration cleanup (m-PFC) method with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with formic acid acetonitrile after being fully wetted with water. QuEChERS salt pack were added to the system to separate into organic and aqueous phases. The upper fraction was purified on an m-PFC column before analysis by LC-MS/MS, the samples were analyzed in multi-reaction monitoring (MRM) mode and quantify by the matrix-matched external standard method. The results showed that 19 sulfonamides had good linearity in the range of 1~100 μg/L with determination coefficients higher than 0.997. The detection limits were in the range of 0.005~0.15 μg/kg, and the quantitation limits were 0.01~0.41 μg/kg. At three spiked levels of 10, 20 and 100 μg/kg, the average recoveries of 19 sulfonamides ranged from 70.0% to 114.1%, with relative standard deviations (RSDs) of 0.5%~9.4%. This method is simple, highly sensitive and reproducible, and is suitable for the detection of sulfonamides in seafood.