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Development and Validation for Simultaneous Determination of Disulfoton and Its Five Metabolites in Seven Agro-Products Using Liquid Chromatography-Tandem Mass Spectrometry Combined with QuEChERS Extraction Method

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Abstract

Disulfoton is highly toxic insecticide and acaricide. Food safety requires analysis of disulfoton and its five metabolites (disulfoton-sulfoxide, disulfoton-sulfone, demeton-S, demeton-S-sulfoxide, and demeton-S-sulfone). However, simultaneous determination of disulfoton and its metabolites in agro-products was not established, and the limits of quantification (LOQs) of reported methods could hardly meet the requirement of maximum residue limits (MRLs) set by some countries or organizations. In the present study, disulfoton and its five metabolites in seven agro-products (maize, oat, rice, pea, asparagus, milk and chicken) were extracted according to a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure and simultaneously determined with a liquid chromatograph tandem-mass spectrometer. The method was accurate and reliable after optimization of several key parameters (chromatographic columns, mobile phase, and clean-up sorbents). The sensitivity of the proposed method was greatly improved through the concentration process. Matrix effects for six analytes in different matrices were evaluated, and matrix-matched calibration standards were used to compensate these matrix enhancement or suppression effects. Under optimal conditions, the developed method showed satisfactory linearity with coefficients of determination (R2) > 0.9919. The limits of detection (LODs) for all target analytes in different agro-products ranged from 0.01 to 1.68 µg/kg, while the LOQs were 5 µg/kg for disulfoton, and 1 µg/kg for its each metabolite. At three fortification levels, the mean recoveries were in the range of 71.3–114.4% with relative standard deviations (RSDs) < 16%. Analysis of 70 market samples showed a trace amount of disulfoton and/or its metabolites in 10% samples. In conclusion, the developed method exhibited both high sensitivity and accuracy, and is suitable and practical for the simultaneous determination of trace levels of disulfoton and its five metabolites in agro-products of plant and animal origin.

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Acknowledgements

This work was supported by Agricultural Science and Technology Innovation Program of Chinese Academy of Agricultural Sciences (CAAS-ZDRW202011) and the USDA Hatch project (HAW05044-R).

Funding

Research grant from Agricultural Science and Technology Innovation Program of Chinese Academy of Agricultural Sciences(CAAS-ZDRW202011) and USDA Hatch project (HAW05044-R).

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Authors and Affiliations

  1. Key Laboratory of Agro-Product Quality and Safety, Ministry of Agriculture and Rural Affairs, Institute of Quality Standards and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing, 100081, People’s Republic of China

    Hui Li, Lingyi Pan, Chunsheng Yu, Xukun Zhang, Xueyan Cui, Ting Luo, Zhen Cao & Jing Wang

  2. Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, Honolulu, HI, 96822, USA

    Qingxiao Li

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  1. Hui Li
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Correspondence to Zhen Cao or Jing Wang.

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Li, H., Pan, L., Yu, C. et al. Development and Validation for Simultaneous Determination of Disulfoton and Its Five Metabolites in Seven Agro-Products Using Liquid Chromatography-Tandem Mass Spectrometry Combined with QuEChERS Extraction Method. Chromatographia 85, 529–537 (2022). https://doi.org/10.1007/s10337-022-04151-1

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