分析测试学报2018，Vol.37Issue(2)：180-189,10.DOI:10.3969/j.issn.1004-4957.2018.02.006
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
摘要
Abstract
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 C18 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/ddMS2 mode under switching positive and negative mode.The calibration curves were linear in the range of 0.5-50 μg/L with correlation coefficients more than 0.998.The limits of quantitation(LOQs) reached to 5 μg/kg.The average recoveries of the analytes at a spiked level of 10 μg/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Key words
on-line cleanup/liquid chromatography/orbitrap high-resolution mass spectrometry/pesticide residues/high-throughput/fruits and vegetables分类
化学化工引用本文复制引用
张海超,艾连峰,马育松,王敬,李晓菲,徐牛生..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[J].分析测试学报,2018,37(2):180-189,10.基金项目
国家质检总局科技计划项目(2013IK154) （2013IK154）
