Chinese Journal of Chromatography ›› 2013, Vol. 31 ›› Issue (9): 850-861.DOI: 10.3724/SP.J.1123.2013.01046

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Determination of 239 pesticide residues in soil by ultra performance liquid chromatography-tandem mass spectrometry

ZHU Yongzhe1, FENG Yanan1, KIM Jeonghan2   

  1. 1. College of Chemistry and Pharmacy, Qingdao Agricultural University, Qingdao 266109, China;
    2. Department of Agricultural Biotechnology, Seoul National University, Seoul 151742, Korea
  • Received:2013-01-25 Revised:2013-03-18 Online:2013-09-28 Published:2013-09-02

Abstract:

A method for the determination of 239 pesticides in soil samples by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) is presented. The sample was prepared with AOAC (Association of Official Analytical Chemists) QuEChERS method for the extraction (acetonitrile, anhydrous MgSO4, CH3COONa). After filtered with a 0.2 μm membrane, the sample was separated and detected by UPLC-MS/MS performing on positive/negative electrospray ionization (ESI+/-) and the multiple reaction monitoring (MRM) mode. In this study, 236 of the 239 pesticides' correlation coefficients were above 0.99, which counted 99% of all the analytes. The limits of detection (LODs) ranged in 0.69-29.04 μg/kg (S/N=3). The recoveries of all the pesticides at 40 μg/kg spiked level were in the range of 50%-150%, and the relative standard deviations (RSDs) were below 20%. In addition, the recoveries of 209 pesticides were in the range of 70%-120%, and RSDs of 161 pesticides were less than 10%. The method is efficient, fast, simple, and accurate. The procedure is suitable for the determination of multi pesticide residues in soil.

Key words: multi-residues, pesticides, QuEChERS, soil, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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