Citation: ZHU Yongzhe, FENG Yanan, KIM Jeonghan. Determination of 239 pesticide residues in soil by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(9): 850-861. doi: 10.3724/SP.J.1123.2013.01046 shu

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

1.
1. College of Chemistry and Pharmacy, Qingdao Agricultural University, Qingdao 266109, China;

Corresponding author: ZHU Yongzhe,
Received Date: 25 January 2013
Available Online: 18 March 2013
Fund Project: 青岛市公共领域科技支撑计划项目(11-2-3-55-nsh) (11-2-3-55-nsh)青岛农业大学高层次人才基金(630608). (630608)

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