在线净化液相色谱-高分辨质谱法快速筛查果蔬中212种农药残留  

Rapid Screening of 212 Pesticide Residues in Fruits and Vegetables by Liquid Chromatography-High Resolution Mass Spectrometry with On-line Cleanup

作　　者：张海超[1] 艾连峰[1] 马育松[1] 王敬[1] 李晓菲 徐牛生 ZHANG Hai-chao;AI Lian-feng;MA Yu-song;WANG Jing;LI Xiao-fei;XU Niu-sheng(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》2018年第2期180-189,共10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筛查果蔬中212种农药残留的方法和数据库。样品经0.1%乙酸乙腈提取,提取液经在线净化柱(Cyclone-P)净化、富集后,以乙腈-0.5 mmol/L乙酸铵(含0.1%乙酸)为流动相梯度洗脱,待测物经C_(18)分析柱色谱分离后,采用四极杆/静电场轨道阱高分辨质谱以正负同时扫描的Full Scan/dd MS2模式进行检测。结果表明,212种农药在0.5~50μg/L范围内呈良好线性,相关系数均大于0.998。方法的定量下限(LOQ)均可达到5μg/kg。通过实际样品的加标回收试验,212种农药在10μg/kg的加标回收率为58.3%~129.4%,相对标准偏差(RSD)为2.8%~16.0%。该方法利用精确质量数、保留时间、同位素峰比、二级碎片等多个定性信息可在无标准物质的情况下实现对果蔬中212种化合物的快速筛查与确证。A new method and mass spectral database for screening pesticide residues in fruits and vegetables by liquid chromatography-high resolution benchtop/orbitrap mass spectrometry(HRMS)with on-line cleanup were developed.The samples were extracted with acetonitrile containing 0.1%acetic acid,then purified and collected with a Cyclone-P column.The analytes were separated on a C 18 column with acetonitrile-0.5 mmol/L ammonium acetate containing 0.1%acetic acid as mobile phase by gradient elution.212 pesticides residues were analyzed by high-resolution mass spectrometry Q-Orbitrap in full scan/ddMS 2 mode under switching positive and negative mode.The calibration curves were linear in the range of 0.5-50μg/L with correlation coefficients more than 0.998.The limits of quantitation(LOQs)reached to 5μg/kg.The average recoveries of the analytes at a spiked level of 10μg/kg were in the range of 58.3%-129.4%,with their relative standard deviations of 2.8%-16.0%.The method could be used for the rapid screening of 212 compounds in fruits and vegetables by means of accurate mass of quasi-molecular ion,retention time,isotope ratio and qualitative fragments without any reference standards.

关 键 词：在线净化 液相色谱 静电场轨道阱高分辨质谱 农药残留 高通量 果蔬 

分 类 号：O657.63[理学—分析化学] O657.7[理学—化学]