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Multiresidue Determination of Fungicides in Wine by Solvent Demulsification-Dispersive Liquid-Liquid Microextraction and Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry

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Abstract

Fungicides are applied from plant development to grape production, transport, and storage. Even after fruit processing, residues of these compounds can be present in grape by-products such as wine and juice. In this way, a fast and straightforward method based on solvent demulsification-dispersive liquid-liquid microextraction (SD-DLLME) sample preparation was developed, validated, and applied for the multiresidue determination of 30 fungicides in wine using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). The evaluated SD-DLLME parameters were agitation types, extraction and dispersive solvent type, extraction and dispersive solvent volume, sample pH, and salt types. Sample preparation using SD-DLLME avoids the centrifugation step. Validation was performed using spiked blank sample and satisfactory results for accuracy, with recoveries ranging from 70 to 117% and precision in terms of relative standard deviation ≤20%, except for three compounds at the lowest spiked level. For most of the compounds, the practical method limits of detection and quantification were 0.03 and 0.1 μg L−1, respectively. The method was successfully applied in commercial wine samples in which several pesticides were found at concentrations ranging from 0.109 to 10.6 μg L−1.

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Acknowledgements

The authors gratefully acknowledge the financial support and fellowships granted by the Brazilian agencies CNPq and CAPES.

Funding

This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - Brazil (CAPES) - Finance Code 001.

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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

    Gabrieli Bernardi, Magali Kemmerich, Franciele F. Machado, Osmar D. Prestes, Martha B. Adaime & Renato Zanella

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  1. Gabrieli Bernardi
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  2. Magali Kemmerich
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  3. Franciele F. Machado
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  4. Osmar D. Prestes
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Correspondence to Renato Zanella.

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This article does not contain any studies with human participants or animals performed by any of the authors. Informed consent was obtained from all individual participants included in the study.

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Gabrieli Bernardi declares that she has no conflict of interest. Magali Kemmerich declares that she has no conflict of interest. Franciele Fátima Machado declares that she has no conflict of interest. Osmar D. Prestes declares that he has no conflict of interest. Martha B. Adaime declares that she has no conflict of interest. Renato Zanella declares that he has no conflict of interest.

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Bernardi, G., Kemmerich, M., Machado, F.F. et al. Multiresidue Determination of Fungicides in Wine by Solvent Demulsification-Dispersive Liquid-Liquid Microextraction and Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry. Food Anal. Methods 15, 2026–2035 (2022). https://doi.org/10.1007/s12161-022-02272-9

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