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


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


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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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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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).

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  • Pesticide residues
  • Sample preparation
  • Food
  • QuEChERS
  • LC-MS/MS