Chinese Journal of Chromatography ›› 2015, Vol. 33 ›› Issue (5): 501-507.DOI: 10.3724/SP.J.1123.2014.12043

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Determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans by QuEChERS-liquid chromatography-tandem mass spectrometry

WANG Lianzhu1, HUANG Xiaoyan1, WANG Dengfei1, CHEN Yong1, XU Dunming2, ZHOU Yu2   

  1. 1. Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363100, China;
    2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China
  • Received:2014-12-30 Published:2015-04-23

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 relative standard deviations of 1.2%-13.0%. The limits of quantification (S/N≥10) were 0.2-5.0 μg/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 soybeans.

Key words: green soybean, liquid chromatography-tandem mass spectrometry (LC-MS/MS), QuEChERS, sulfonylurea herbicide, sweet corn, zirconium dioxide

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