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A method for the determination of 70 pesticides in extra virgin olive oil based on a limited-volume solvent extraction step prior to comprehensive two-dimensional gas chromatography-tandem mass spectrometry

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Abstract

The goal of the present research was to develop a method based on a miniaturized solvent extraction step (using only 500 μL of acetonitrile, with no further clean-up or concentration processes) prior to cryogenic-modulation comprehensive two-dimensional gas chromatography-tandem mass spectrometry for the determination of seventy pesticides in extra virgin olive oil, exploiting the enhanced specificity and sensitivity of this technique. Limits of quantification were always below European legislation residue limits, intra-day precision was between 0.3 and 4.9% (at the 50 and 100 μg kg−1 concentration levels), inter-day precision was between 1.6 and 6.1% (at the 100 μg kg−1 concentration level), recovery (at the 20, 50, and 100 μg kg−1 concentration levels) was in the 14–120% range, accuracy at the initial stage of the work (within repeatability conditions) was between 79 and 110%, while accuracy after 3 months (within intermediate precision conditions) was between 91 and 121% (at the 50 and 100 μg kg−1 concentration levels). Finally, the matrix effect was always positive, between 16 and 197%. The method was applied to the investigation of twenty samples, and eleven of these were found to be contaminated.

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Acknowledgements

The authors gratefully acknowledge the Shimadzu Corporation and Merck Life Science for their continuous support.

“This article is based upon work from the Sample Preparation Task Force and Network, supported by the Division of Analytical Chemistry of the European Chemical Society.”

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Authors and Affiliations

  1. Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy

    Alessia Arena, Luigi Mondello & Peter Q. Tranchida

  2. Department of Mathematical and Computer Science, Physical Sciences and Earth Sciences, University of Messina, Messina, Italy

    Mariosimone Zoccali

  3. Chromaleont S.R.L., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy

    Luigi Mondello

  4. Department of Sciences and Technologies for Human and Environment, University Campus Bio-Medico of Rome, Rome, Italy

    Luigi Mondello

Authors
  1. Alessia Arena
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  2. Mariosimone Zoccali
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  3. Luigi Mondello
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  4. Peter Q. Tranchida
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Contributions

AA: conceptualization, methodology, validation, writing — original draft. MZ: conceptualization, methodology, supervision, writing — original draft, writing — review and editing. LM: conceptualization, funding acquisition, resources, writing — review and editing. PQT: conceptualization, writing — original draft, writing — review and editing.

Corresponding author

Correspondence to Mariosimone Zoccali.

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Competing interests

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. The author Luigi Mondello is an editor of this journal but was not involved in the peer review of this article.

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Published in the topical collection Comprehensive 2D Chromatography with guest editors Peter Q. Tranchida and Luigi Mondello.

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Arena, A., Zoccali, M., Mondello, L. et al. A method for the determination of 70 pesticides in extra virgin olive oil based on a limited-volume solvent extraction step prior to comprehensive two-dimensional gas chromatography-tandem mass spectrometry. Anal Bioanal Chem 415, 2459–2469 (2023). https://doi.org/10.1007/s00216-022-04494-6

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  • DOI: https://doi.org/10.1007/s00216-022-04494-6

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