液相色谱-电喷雾串联四极杆质谱法测定鸡肉中17种磺胺类药物的残留

Simultaneous Determination of Seventeen Sulfonamide Residues in Chickens by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

建立了鸡肉中17种磺胺类药物残留量的液相色谱-电喷雾串联四极杆质谱测定方法.以稳定同位素13C6-磺胺二甲基嘧啶作为内标,采用多反应监测定量.样品经过匀浆、乙腈提取、正己烷脱脂、硅胶柱净化后进行液相色谱-质谱分析.采用Capcell Pak C8DD色谱柱,以均含0.2%甲酸的水和甲醇为流动相进行梯度洗脱.方法检出限为0.02～1 μg/kg,17种磺胺类药物的加标回收率为52.3% ～124.9% (添加水平为1,5,10 μg/kg),相对标准偏差为1.0% ～17.6% .

A liquid chromatography-electrospray tandem mass spectrometry （LC-MS/MS） for the simultaneous determination of seventeen commonly used sulfonamide （SA） residues in chickens has been developed. Stable isotopic compound ^13C6-sulfamethazine was used as internal standard. Multi-reaction monitoring mode was employed for the quantitative determination.The separation was performed on a Capcell Pak C8 DD column （ 150 mm ×2.0 mm i. d. , 5 μm）with a gradient system of water （ containing 0.2% formic acid ）-methanol （ containing 0.2% formic acid） as mobile phase at a flow rate of 0.2 mL/min. Samples were prepared by homogenizing the chicken, extracting with acetonitrile, defatting with n-hexane and cleaning-up with Sep-Pak Silica solid-phase extraction. The detection limits of 0.02 - 1 μg/kg proved to be much better than the previously reported ones. Average recoveries of seventeen SAs （spiked at the levels of 1, 5, l0 μg/kg） ranged from 52.3% to 124.9%, with relative standard deviations between 1.0% and 17.6%. Intra-day and inter-day variations of the method were all with in the acceptable ranges. The results demonstrated that the method is simple, accurate and suitable for the identification and quantification of these sulfonamide residues in chickens.