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A multiresidue method for the analysis of 90 pesticides, 16 PAHs, and 22 PCBs in honey using QuEChERS–SPME

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Abstract

An optimized analytical method was developed for the simultaneous analysis of 90 pesticides, 16 polycyclic aromatic hydrocarbons, and 22 polychlorinated biphenyls. The method was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction using acetonitrile followed by a dispersive solid-phase extraction cleanup using primary–secondary amine and octadecyl (C18). The extract obtained was concentrated by evaporation and then reconstituted with acetonitrile to prepare it for chromatographic analysis by liquid chromatography–triple-quadrupole tandem mass spectrometry and gas chromatography–ion-trap tandem mass spectrometry, which was preceded by a preconcentration step using solid-phase microextraction with appropriate fibers. The combination of the two extraction steps ensured efficient extract cleanup. The use of the two analytical instruments allowed the analysis of a large number of pollutants with a high reliability rate. The method developed was validated for linearity, which was studied with use of matrix-matched calibration curves in the concentration range between 10 and 3000 ng g−1. The correlation coefficient (R 2) obtained was higher than 0.98 for most of the target compounds, with a relative standard deviation lower than 20% for repeatability and reproducibility. The limits of detection and quantification were lower than 20 and 60 ng g-1 respectively for the compounds analyzed, and the recoveries were between 60% and 103% for most compounds. Finally, the method was tested for its efficiency on real samples by the analysis of three honey samples in which seven pesticides and nine polycyclic aromatic hydrocarbons were determined.

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Acknowledgements

We gratefully acknowledge AZM & SAADE Association and the Lebanese University for funding the project, as well as Strasbourg University for international mobility aid, without which the present study could not have been completed.

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Authors and Affiliations

  1. Laboratory of Applied Biotechnology, Azm Center for Research in Biotechnology and Its Applications, Doctoral School of Science and Technology, Lebanese University, El Mittein Street, 1300, Tripoli, Lebanon

    Josephine Al-Alam, Ziad Fajloun & Asma Chbani

  2. Institute of Chemistry and Processes for Energy, Environment and Health ICPEES UMR 7515 Group of Physical Chemistry of the Atmosphere, University of Strasbourg, 1, rue Blessig, 67084, Strasbourg, France

    Josephine Al-Alam & Maurice Millet

  3. Faculty of Sciences III, Lebanese University, 1300, Tripoli, Lebanon

    Ziad Fajloun

  4. Faculty of Public Health III, Lebanese University, 1300, Tripoli, Lebanon

    Asma Chbani

Authors
  1. Josephine Al-Alam
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  2. Ziad Fajloun
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  4. Maurice Millet
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Correspondence to Maurice Millet.

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Al-Alam, J., Fajloun, Z., Chbani, A. et al. A multiresidue method for the analysis of 90 pesticides, 16 PAHs, and 22 PCBs in honey using QuEChERS–SPME. Anal Bioanal Chem 409, 5157–5169 (2017). https://doi.org/10.1007/s00216-017-0463-y

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  • DOI: https://doi.org/10.1007/s00216-017-0463-y

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