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Simultaneous determination of chlorpyrifos and 3,5,6-trichloro-2-pyridinol in duck muscle by modified QuEChERS coupled to gas chromatography tandem mass spectrometry (GC-MS/MS)

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Abstract

A rapid, specific, and sensitive method based on modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) coupled to gas chromatography tandem mass spectrometry (GC-MS/MS) was developed and validated for simultaneous determination of chlorpyrifos (CP) and its metabolite 3,5,6-trichloro-2-pyridinol (TCP) in duck muscle. The residues of CP and TCP were extracted by acidified acetonitrile. The fat layer of the extract was removed under −20 °C, then the organic layer was evaporated. The analytes were derivatized by N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) and cleaned up by a mixture of 150 mg MgSO4, 25 mg graphitized carbon black (GCB), and 50 mg N-propylethylenediamine (PSA) to remove interference. The final extract was analyzed by GC-MS/MS. Recovery values at the spiking concentrations ranged from 86.2 to 92.3 % for CP and from 74.8 to 81.8 % for TCP, with relative standard deviations (RSDs) lower than 9.5 and 12.3, respectively. The correlation coefficients of CP (from 2 to 2,000 μg/kg) and TCP (from 1 to 1,000 μg/kg) were equal to or higher than 0.998. The limits of detection (LODs) were 0.3 and 0.15 μg/kg, and the limits of quantification (LOQs) were 1.0 and 0.5 μg/kg for CP and TCP in duck muscle, respectively. The average intra- and inter-day accuracy ranged from 84.6 to 91.2 % for CP and 75.6 to 82.3 % for TCP, and the intra- and inter-day precisions were from 5.8 to 8.2 % for CP and 6.5 to 11.9 % for TCP. Furthermore, the CP and TCP residues in duck muscle samples were detected for dietary risk assessment using the validated method.

Simultaneous determination of chlorpyrifos and 3,5,6-trichloro-2-pyridinol residues in duck muscle

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Acknowledgements

This work was supported by grants from Zhejiang Provincial Science and Technology Project (2011C12024), International Cooperation Project of Ministry of Science and Technology (2013DFA31450) and International Cooperation Project of Zhejiang Province (2013C24021).

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Authors and Affiliations

  1. State Key Laboratory Breeding Base for Zhejiang Sustainable Plant Pest Control; Agricultural Ministry Key Laboratory for Pesticide Residue Detection; Zhejiang Province Key Laboratory for Food Safety; Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, 310021, Hangzhou, Zhejiang, China

    Rui Li, Xiaofeng Ji, Mingrong Qian, Yu Zhou & Qiang Wang

  2. National Shanghai Center for New Drug Safety Evaluation and Research, 201203, Shanghai, China

    Liang He

  3. Guelph Food Research Centre, Agriculture and Agri-Food Canada, 93 Stone Road West, Guelph, ON, N1G 5C9, Canada

    Ting Zhou

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  1. Rui Li
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  2. Liang He
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  3. Ting Zhou
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  4. Xiaofeng Ji
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  6. Yu Zhou
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Correspondence to Yu Zhou or Qiang Wang.

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Li, R., He, L., Zhou, T. et al. Simultaneous determination of chlorpyrifos and 3,5,6-trichloro-2-pyridinol in duck muscle by modified QuEChERS coupled to gas chromatography tandem mass spectrometry (GC-MS/MS). Anal Bioanal Chem 406, 2899–2907 (2014). https://doi.org/10.1007/s00216-014-7717-8

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  • DOI: https://doi.org/10.1007/s00216-014-7717-8

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