色谱Issue(5)：501-507,7.DOI:10.3724/SP.J.1123.2014.12043
QuEChERS-液相色谱-串联质谱法测定甜玉米及毛豆中32种磺酰脲类除草剂残留
Determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans by QuEChERS-liquid chromatography-tandem mass spectrometry
摘要
Abstract
A fast method based on QuEChERS methodology for the simultaneous determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans was developed using liquid chromatography-tandem mass spectrometry( LC-MS/MS). The clean-up effects of three dispersive sorbents were evaluated in terms of the residue mass for extracts after evaporation and recoveries. The three sorbents were C18,a mixture of two sorbents silica coated with zirconium dioxide( Z-Sep)and C18,a bonded C18 zirconia-coated silica( Z-Sep+). As a result, the best effects were obtained from using Z-Sep/C18 sorbents. The samples were extracted with acetonitrile,and salted out with anhydrous magnesium sulphate and sodium chloride. The extracts were cleaned up with dispersive solid phase extraction using Z-Sep/C18 sorbents. Chromatographic analysis was carried out using a CSH C18 column with gradient elution. The pesticides were analyzed by negative electrospray ionization tandem mass spectrometry under scheduled multiple reaction monitoring mode. The quantification was achieved using matrix-matched standard calibrations as the external standard. The recoveries at fortification levels of 10,20,100 μg/kg in sweet corns and green beans ranged from 80. 0% to 108. 2% with the rela-tive standard deviations of 1. 2%-13. 0%. The limits of quantification( S/N≥10)were 0. 2-5. 0μg/kg. The method has been proven to be simple,sensitive,environmental,and thus suitable for the determination of the 32 sulfonylurea herbicide residues in sweet corns and green soy-beans.关键词
QuEChERS/氧化锆/液相色谱-串联质谱/磺酰脲类除草剂/甜玉米/毛豆Key words
QuEChERS/zirconium dioxide/liquid chromatography-tandem mass spectrometry(LC-MS/MS)/sulfonylurea herbicide/sweet corn/green soybean分类
化学化工引用本文复制引用
王连珠,黄小燕,王登飞,陈泳,徐敦明,周昱..QuEChERS-液相色谱-串联质谱法测定甜玉米及毛豆中32种磺酰脲类除草剂残留[J].色谱,2015,(5):501-507,7.基金项目
福建省自然科学基金项目（2011J01386）． （）
