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Ultrasound-assisted QuEChERS-based extraction using EDTA for determination of currently-used pesticides at trace levels in soil

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Abstract

It is essential to monitor pesticides in soils as their presence at trace levels and their bioavailability can induce adverse effects on soil’s ecosystems, animals, and human health. In this study, we developed an analytical method for the quantification of traces of multi-class pesticides in soil using liquid chromatography-tandem mass spectrometry. In this way, 31 pesticides were selected, including 12 herbicides, 9 insecticides, and 10 fungicides. Two extraction techniques were first evaluated, namely, the pressurized liquid extraction and the QuEChERS procedure. The latest one was finally selected and optimized, allowing extraction recoveries of 55 to 118%. The role of the chelating agent EDTA, which binds preferentially to soil cations that complex some pesticides, was highlighted. Coupled with liquid chromatography-tandem mass spectrometry, the procedure displayed very high sensitivity, with limits of quantification (LOQ) in the range 0.01–5.5 ng/g. A good linearity (R2 > 0.992) was observed over two orders of magnitude (LOQ-100 \(\times\) LOQ) with good accuracy (80–120%) for all compounds except the two pyrethroids lambda-cyhalothrin and tau-fluvalinate (accuracy comprised between 50 and 175%) and the cyclohexanedione cycloxydim (accuracy < 35%). Good repeatability and reproducibility were also achieved. The method was finally successfully applied to 12 soil samples collected from 3 land-use types. Among the 31-targeted pesticides, 24 were detected at least once, with concentration levels varying from LOQ to 722 ng/g. Many values were below 0.5 ng/g, indicating that the developed method could provide new knowledge on the extremely low residual contents of some pesticides.

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Acknowledgements

The authors would like to thank the “Zone Atelier Plaine et Val de Sèvre” and especially Vincent Bretagnolle for the study site access and provision of site infrastructures. They also thank all the people who took part in the soil sampling in Chizé.

Funding

This work has been financially supported by the French OFB (Office Français de la Biodiversité, formerly ONEMA) within the national call “Pesticides” (APR ECOPHYTO 2014).

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Authors and Affiliations

  1. Univ Lyon, CNRS, Université Claude Bernard Lyon 1, Institut Des Sciences Analytiques, UMR 5280, 5 rue de la Doua, 69100, Villeurbanne, France

    Florent Lafay, Gaëlle Daniele, Maëva Fieu & Emmanuelle Vulliet

  2. INRAe, Avignon Université, UMR EMMAH, 84000, Avignon, France

    Céline Pelosi

  3. INRAe, UMR1402 ECOSYS, pôle Ecotoxicologie Ecologie fonctionnelle et écotoxicologie des agroécosystèmes, RD 10 Route de St Cyr, 78026, Versailles Cedex, France

    Céline Pelosi

  4. UMR 6249 Chrono-Environnement – CNRS/Université Bourgogne Franche-Comté Usc INRA - 16 Route de Gray, 25030, Besancon Cedex, France

    Clémentine Fritsch

Authors
  1. Florent Lafay
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  2. Gaëlle Daniele
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  3. Maëva Fieu
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  4. Céline Pelosi
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  5. Clémentine Fritsch
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  6. Emmanuelle Vulliet
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Contributions

FL and MF carried out the analytical work. GD and EV supervised the analytical development. GD wrote the original draft. CP and CF coordinated the research project and selected and organized the soil sampling. All authors read and approved the final manuscript.

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Correspondence to Gaëlle Daniele.

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Lafay, F., Daniele, G., Fieu, M. et al. Ultrasound-assisted QuEChERS-based extraction using EDTA for determination of currently-used pesticides at trace levels in soil. Environ Sci Pollut Res (2022). https://doi.org/10.1007/s11356-022-19397-3

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