色谱2016，Vol.34Issue(7)：686-691,6.DOI:10.3724/SP.J.1123.2016.04017
QuEChERS-液相色谱-串联质谱法测定棕榈原油中敌草快等6种农药残留
Determination of six pesticide residues including diquat in crude palm oil by QuEChERS-liquid chromatography-tandem mass spectrometry
摘要
Abstract
A fast method based on QuEChERS methodology was developed for the simultane-ous determination of diquat, dimethoate, fenthion, fenthion-sulfoxide, fenthion-sulfone, haloxyfop-methyl in crude palm oil using liquid chromatography-tandem mass spectrometry ( LC-MS/MS). The clean-up effects of four dispersive sorbents were evaluated in terms of recoveries and matrix effects. The four sorbents were the mixture of primary secondary amine ( PSA)and C18,a mixture of two sorbents a bonded C18 zirconia-coated silica( Z-Sep+) and C18,Z-Sep+,C18. As a result,the best effects were obtained from using the mixture of Z-Sep+ and C18 sorbents. The samples were extracted with methanol containing 1%( v/v ) acetic acid. The extracts were cleaned up with dispersive solid phase extraction using Z-Sep+/C18 sorbents. Chromatographic analysis was carried out on an Atlantis T3 column with gradient elution. The pesticides were analyzed by positive electrospray ionization-tandem mass spec-trometry under multiple reaction monitoring mode. The quantification was achieved using matrix-matched standard calibrations as external standard. The recoveries at the fortification levels of 10,20 and 250 μg/kg in crude palm oil ranged from 70. 0% to 97. 9% with the relative standard deviations of 2. 6%-10. 2%. The limits of quantification( S/N≥10 ) were 0. 1-2. 5μg/kg. The method has been proven to be simple,sensitive,accurate and environmental and thus suitable for the determination of the six pesticide residues above in crude palm oil.关键词
QuEChERS/液相色谱-串联质谱/敌草快/农药残留/棕榈原油/氧化锆Key words
QuEChERS/liquid chromatography-tandem mass spectrometry (LC-MS/MS)/diquat/pesticide residues/crude palm oil/zirconium dioxide分类
化学化工引用本文复制引用
王连珠,李晓莲,方恩华,陈泳,王登飞,徐敦明..QuEChERS-液相色谱-串联质谱法测定棕榈原油中敌草快等6种农药残留[J].色谱,2016,34(7):686-691,6.基金项目
福建省自然科学基金项目（2011J01386，2016J01070）．@@@@Fujian Provincial Natural Science Foundation（ Nos．2011J01386，2016J01070）． （）
