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分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留

周蓉 曹赵云 赵肖华 林晓燕 牟仁祥

分析测试学报2017,Vol.36Issue(1):67-72,6.
分析测试学报2017,Vol.36Issue(1):67-72,6.DOI:10.3969/j.issn.1004-4957.2017.01.011

分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留

Determination of Nineteen Organophosphorus Pesticides in Vegetables by Gas Chromatography-Tandem Mass Spectrometry Combined with Dispersive Solid-phase Extraction and Dispersive Liquid-Liquid Micro-extraction

周蓉 1曹赵云 1赵肖华 1林晓燕 1牟仁祥1

作者信息

  • 1. 中国水稻研究所农业部稻米及制品质量监督检验测试中心,浙江杭州310006
  • 折叠

摘要

Abstract

A gas chromatograpy-tandem mass spectrometric (GC-MS/MS) method for the determination of nineteen organophosphorus pesticides in vegetables was developed using dispersive solidphase extraction(DSPE) and dispersive liquid-liquid micro-extraction (DLLME) as sample preparation methods.With dispersive solid-phase extraction,PSA and C18 were used as the sorbents,and acetonitrile as the eluted solvent.Some experimental parameters influencing the extraction efficiency,such as the types and volume of the dispersive solvents and extraction solvents were examined and optimized.Gamma-L-gulonic acid lactone(AP) used as a masking regent for compensation effect of matrix was evaluated.Under the optimum conditions,the recoveries of nineteen organophosphorus pesticides in pepper chili and shallot samples at fortified levels of 0.05,0.1,0.5 mg/kg ranged from 76.9% to 126.8% with relative standard deviations of 0.6%-7.3%.The limits of detection(S/N =3) were in the range of 0.10-0.50 μg/kg.With the advantages of quickness,low toxicity and high enrichment factors,the proposed method is applicable for the analysis of organophosphorus pesticides in vegetables.

关键词

分散液液微萃取/分散固相萃取/气相色谱-串联质谱(GC-MS/MS)/有机磷/蔬菜

Key words

dispersive liquid-liquid micro-extraction/dispersive solid-phase extraction/gas chromatography-tandem mass spectrometry(GC-MS/MS)/organophosphorus pesticides/vegetables

分类

化学化工

引用本文复制引用

周蓉,曹赵云,赵肖华,林晓燕,牟仁祥..分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留[J].分析测试学报,2017,36(1):67-72,6.

基金项目

浙江省科技计划项目(2015C37057) (2015C37057)

分析测试学报

OA北大核心CSCDCSTPCD

1004-4957

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