色谱Issue(4):408-412,5.DOI:10.3724/SP.J.1123.2014.12016
基质分散固相萃取-超高效液相色谱-串联质谱法测定蔬菜风险监测中的9种农药残留
Determination of nine pesticide residues in vegetables by matrix solid-phase dispersion-ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A matrix solid⁃phase dispersion⁃ultra performance liquid chromatography⁃tandem mass spectrometry ( MSPD⁃UPLC⁃MS/MS) method was established for the simultaneous deter⁃mination of carbendiazin, omethoate, carbofuran, aldicarb, chlorpyrifos, methamidophos, phorate, parathion and parathion⁃methyl residues in vegetables. The samples were extracted by acetonitrile and separated with salting out method. And then the supernatants were purified by matrix solid⁃phase dispersion for the UPLC⁃MS/MS analysis. The separation was performed on a Waters Acquity UPLC system with a BEH C18 column with the gradient elution of acetonitrile and water containing 0�1%( v/v) acetic acid. The nine pesticides were determined in the modes of electrospray positive ionization ( ESI+) and multiple reaction monitoring ( MRM ) . The ana⁃lytes were quantified by matrix matched standard solution curves. The limits of detection ( S/N≥3) were 0�8-4�0 μg/kg. The average recoveries were 72. 8%-117. 4%. The detection rates were 42�0% for chlorpyrifos, 14�0% for carbendiazin and 1�5% for dimethoate, and the exces⁃sive rate of chlorpyrifos was 8�0% in the determination of 50 real samples;the other pesticides were not detected. The method is simple, accurate and highly reproducible. This method is suit⁃able for the quality control of pesticide residues in risk monitoring of the safety of the foods.关键词
基质分散固相萃取/超高效液相色谱-串联质谱/农药残留/风险监测/蔬菜Key words
matrix solid-phase dispersion (MSPD)/ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/pesticide residues/risk monitoring/vegetables分类
化学化工引用本文复制引用
巩丽萍,石峰,姜树银,赵艳霞,郭常川..基质分散固相萃取-超高效液相色谱-串联质谱法测定蔬菜风险监测中的9种农药残留[J].色谱,2015,(4):408-412,5.基金项目
国家食品安全风险监测计划项目(中检办食化函[2013]50号). ()