在线净化液相色谱-高分辨质谱法快速测定动物源性食品中均三嗪类药物及其代谢产物的残留量  

Rapid Determination of Diclazuril,Toltrazuril and Their Metabolite Residues in Foods of Animal Origin by On-line Cleanup Liquid Chromatography-High Resolution Mass Spectrometry

作　　者：张海超[1] 马育松[1] 李颖[1] 艾连峰[1] 徐牛生 陈瑞春[1] 郭春海[1] ZHANG Hai-chao MA Yu-song LI Ying AI Lian-feng XU Niu-sheng CHEN Rui-chun GUO Chun-hai(Hebei Entry and Exit Inspection and Quarantine Bureau, Shijiazhuang 050051, China Thermo Fisher Scientific （China）, Shanghai 201206, China)

机构地区：[1]河北出入境检验检疫局,河北石家庄050051 [2]赛默飞世尔科技(中国)有限公司,上海201206

出　　处：《分析测试学报》2017年第3期331-336,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2013IK154)

摘　　要：基于在线净化液相色谱-四极杆/静电场轨道阱高分辨质谱技术建立了快速测定动物源食品中地克珠利、妥曲珠利、妥曲珠利砜和妥曲珠利亚砜残留的分析方法。样品采用乙腈提取,经Cyclone在线净化柱净化后,将富集的目标物洗脱转至C_(18)分析柱,经色谱分离后,采用四极杆/静电场轨道阱高分辨质谱以Full Scan/dd MS2模式进行检测。4种化合物在0.5~50 ng/m L范围内呈良好线性,相关系数均大于0.999 4,方法的定量下限(LOQ)为2μg/kg。待测物在4种基质中的加标回收率为80.2%~110.5%,相对标准偏差为2.8%~9.7%。该方法简化了前处理过程,消除了基质干扰。利用精确质量数、保留时间、同位素峰比、二级碎片多个定性信息能够实现快速确证测定。A new method was developed for the rapid determination of diclazuril,toltrazuril,toltrazurilsulfone and toltrazurilsulfoxide residues in foods of animal origin by on line cleanup liquid chromatography-high resolution benchtop quadropole/obitrap mass spectrometry（HRMS） .The samples were extracted with acetonitrile,and purified on a Cyclone column.The analytes were eluted from the exaction column and put into a C18 analytical column prior to chromatographic separation and detection in full scan/ddMS^2 mode.The calibration curves were linear in the range of 0.5-50 ng/mL with correlation coefficients more than 0.999 4.The limits of quantitation（LOQ） were 2 μg/kg.Average recoveries of the analytes in four matrices ranged from 80.2% to 110.5%,with relative standard deviations of 2.8%-9.7%.With simple pretreatment,low matrix effects,this method could be used for the rapid confirmation with accurate mass of quasi molecular ion,retention time,isotope ratio and qualitative fragments.

关 键 词：在线净化 静电场轨道阱高分辨质谱 地克珠利 妥曲珠利 妥曲珠利亚砜 妥曲珠利砜 动物源食品 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]