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Methodology for trace analysis of 17 pyrethroids and chlorpyrifos in foodstuff by gas chromatography–tandem mass spectrometry

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Abstract

This study aimed to develop an efficient, sensitive, and reliable analytical method for trace analysis of 17 different pyrethroids and chlorpyrifos in the fatty content of animal products, including beef, chicken, eggs, fish, and milk. The method developed is based on an ultrasound extraction using lyophilized samples, a solid phase extraction cleanup with basic alumina and C18 cartridges in tandem, and analysis by gas chromatography coupled to tandem mass spectrometry in negative chemical ionization mode. Recovery values were in the range of 27–128 % with relative standard deviation always below 25 %, and chiral analysis of recovery data showed predominance of isomers of cis form over trans. Limits of detection (LODs) ranged from 0.002 to 6.43 ng g−1 lipid weight (lw), and limits of quantification (LOQs) ranged between 0.006 and 21.4 ng g−1 lw. The developed methodology was used for the analysis of 25 samples of fatty foods. All samples were positive for at least one of the pesticides, chlorpyrifos, bifenthrin, cyhalothrin, permethrin, cypermethrin, or deltamethrin, with mass fraction levels ranging from 0.03 to 270 ng g−1 lw.

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Acknowledgments

This research was funded by the CAPES, CNPq and Ministerio da Agricultura. To Ciencias sem Fronteiras, CAPES, for the sandwich scholarship, for Alexsandro Dallegrave. This work has also been supported by the Generalitat de Catalunya (Consolidated Research Groups “2014 SGR 418 - Water and Soil Quality Unit”). Biotage is acknowledged for SPE cartridges.

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Authors and Affiliations

  1. Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS, Avenida Bento Gonçalves 6500, Porto Alegre, Rio Grande do Sul, 91501-970, Brazil

    Alexsandro Dallegrave & Tânia Mara Pizzolato

  2. Laboratório Nacional Agropecuário - LANAGRO/RS, Estrada da Ponta Grossa 3036, Porto Alegre, Rio Grande do Sul, 91780-580, Brazil

    Fabiano Barreto

  3. Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18-26, 08034, Barcelona, Spain

    Ethel Eljarrat & Damià Barceló

Authors
  1. Alexsandro Dallegrave
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  2. Tânia Mara Pizzolato
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  3. Fabiano Barreto
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  4. Ethel Eljarrat
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  5. Damià Barceló
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Correspondence to Tânia Mara Pizzolato.

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Dallegrave, A., Pizzolato, T.M., Barreto, F. et al. Methodology for trace analysis of 17 pyrethroids and chlorpyrifos in foodstuff by gas chromatography–tandem mass spectrometry. Anal Bioanal Chem 408, 7689–7697 (2016). https://doi.org/10.1007/s00216-016-9865-5

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  • DOI: https://doi.org/10.1007/s00216-016-9865-5

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