Chinese Journal of Chromatography ›› 2009, Vol. 27 ›› Issue (4): 391-400.

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Determination of 107 pesticide residues in vegetables using off-line dispersive solid-phase extraction and gas chromatography-tandem mass spectrometry

SHEN Weijian1*, YU Keyao1, GUI Qianwen1, JIANG Yuan1, ZHAO Zengyun1, SHEN Chongyu1, WU Bin1, CHU Xiaogang2   

  1. 1.Food Laboratory of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2.Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • Received:2009-02-18 Revised:2009-04-17 Online:2009-07-30 Published:1982-06-25
  • Contact: SHEN Weijian

Abstract: A screening method was developed for the determination of 107 pesticide residues in vegetables using off-line dispersive solid-phase extraction (DSPE) and gas chromatography-tandem mass spectrometry (GC-MS/MS). The pesticides interested were extracted from the samples with acetonitrile (saturated by n-hexane) containing 1% acetic acid and simultaneously separated by liquid-liquid partitioning with adding anhydrous magnesium sulfate plus sodium acetate following by a simple cleanup step known as dispersive solid-phase extraction. The extracts were determined by GC-MS/MS using external standard method. The method was reliable and stable that the recoveries of almost all pesticides were in the range from 60% to 130% at the spiked level of 10 μg/kg into four vegetable matrixes (garlic, green bean, radish and spinach) and the relative standard deviations (RSDs) were all not more than 15.3%. The linearity of the method was good between 0.05 mg/L and 1 mg/L, and all limits of quantification (LOQs) less than 10 μg/kg. The method is selective with no interference, especially in the complicated garlic matrix.

Key words: dispersive solid-phase extraction (DSPE), gas chromatography-tandem mass spectrometry (GC-MS/MS), multiple pesticide residues, selected reaction monitoring (SRM), vegetables