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Modified QuEChERS Method for Multiresidue Determination of Pesticides in Pecan Nuts by Liquid Chromatography Tandem Mass Spectrometry

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Abstract

Pecan nut is a crop of growing economic importance with a worldwide production around 124,000 tons during the 2017/2018 harvest. Thus, a simple and fast method for the determination of pesticide residues in this crop based on a QuEChERS sample preparation procedure and liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis was developed and validated. Despite the complexity of this matrix, with high fat content, the method was suitable to analyze 47 compounds in pecan nuts employing original QuEChERS salts and clean-up with the sorbents PSA and C18. This combination showed best results for lipid removal and compound recoveries when compared with the sorbents Z-Sep+, EMR-Lipid®, chitosan, diatomaceous earth, silica, and Florisil®. Validation was performed according to SANTE guideline using blank samples spiked at 5, 10, 20, 50, and 100 μg kg−1, and the proposed method presented satisfactory results with recoveries for most of the pesticides in the range of 70–120% with RSD < 20% and practical limits of quantification from 5 to 10 μg kg−1 for all compounds. The method was successfully applied in real samples and demonstrated to be simple, robust, and effective to be applied in routine analysis.

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Acknowledgments

Particular words of gratitude are owed to Martha B. Adaime for her support and helpful comments.

Funding

This study was financed in part by the financial support and fellowships granted by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - Brasil (CAPES) - Finance Code 001 and CNPq.

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Authors and Affiliations

  1. Laboratory of Pesticide Residues Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900, Brazil

    Paulo E. P. Barci, Larissa da S. Alves, Állisson A. S. Avellar, Lucila R. Cendon, Pimpernelli J. dos Santos, Fabiane M. Stringhini, Osmar D. Prestes & Renato Zanella

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  1. Paulo E. P. Barci
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  2. Larissa da S. Alves
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  3. Állisson A. S. Avellar
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  4. Lucila R. Cendon
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  5. Pimpernelli J. dos Santos
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  6. Fabiane M. Stringhini
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  7. Osmar D. Prestes
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  8. Renato Zanella
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Corresponding author

Correspondence to Renato Zanella.

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Conflict of Interest

Paulo E. P. Barci declares that he has no conflict of interest. Larissa da S. Alves declares that she has no conflict of interest. Állisson A. S. Avellar declares that he has no conflict of interest. Lucila R. Cendon declares that she has no conflict of interest. Pimpernelli J. dos Santos declares that she has no conflict of interest. Fabiane M. Stringhini declares that she has no conflict of interest. Osmar D. Prestes declares that he has no conflict of interest. Renato Zanella declares that he has no conflict of interest.

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This article does not contain any studies with human participants or animals performed by any of the authors.

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Barci, P.E.P., Alves, L.d.S., Avellar, Á.A.S. et al. Modified QuEChERS Method for Multiresidue Determination of Pesticides in Pecan Nuts by Liquid Chromatography Tandem Mass Spectrometry. Food Anal. Methods 13, 793–801 (2020). https://doi.org/10.1007/s12161-019-01696-0

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  • DOI: https://doi.org/10.1007/s12161-019-01696-0

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