UPLC-MS/MS检测鸡蛋中16种磺胺类药物残留  

Simultaneous determination of sixteen sulfonamides residues in eggs using liquid chromatography coupled with electrospray ionization tandem mass spectrometry

作　　者：刘洪斌[1] 姚喜梅 蔡英华[1] 姜艳彬[1] 于雷[1] 

机构地区：[1]中国动物疫病预防控制中心,北京100125 [2]中国标准化协会,北京100048

出　　处：《分析试验室》2015年第10期1141-1144,共4页Chinese Journal of Analysis Laboratory

基　　金：十二五国家科技支撑计划项目(2014BAD13B05)资助

摘　　要：采用UPLC-MS/MS建立了鸡蛋中16种磺胺类药物残留检测方法。样品经过磷酸盐缓冲液提取、正己烷分步去脂,氮吹、MCX柱净化后,经Acquity UPLC BEH（100 mm×2.1 mm,1.7μm）分离,以甲醇和0.1%加酸水溶液为流动相进行梯度洗脱,16种化合物能在11 min完全分离,方法的定量限均低于1.0μg/kg,在2.5~100μg/L范围内,16种磺胺类药物线性良好,相关系数均在0.99以上;通过2,10,40μg/kg加标回收实验表明,回收率为62.7%~96.1%,RSD为2.1%~15%。方法满足鸡蛋中磺胺类药物残留检测要求。A multi-residue method based on ultra performance liquid chromatography tandem mass spectrometry has been developed for the detection of sixteen sulfonamides residues in eggs. In this method,analytes were extracted by phosphate buffer,degreased by n-hexane,and purified by MCX SPE column. Sixteen sulfonamides were analyzed by Acquity UPLC BEH C18 column（ 100 mm × 2. 1 mm,1. 7 μm） using methanol and 0. 1%formic acid in water as the mobile phases. All analytes could be well-separated by a gradient program during eleven minutes. The calibration curves of sixteen sulfonamides were linear in a concentration range of 2. 5 ~100 μg / L（ r〉0. 99）,and the limits of quantitation were all less than 1. 0 μg / kg. The recoveries of 2,10 and40 μg / kg spiked samples ranged from 62. 7% to 96. 1%,with RSDs of 2. 1% ~ 15%. This method can satisfy the detection requirements of sulfonamides residues in eggs.

关 键 词：鸡蛋 磺胺类 UPLC-MS/MS 

分 类 号：R917[医药卫生—药物分析学]