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Methodology development based on “dilute and shoot” and QuEChERS for determination of multiple mycotoxins in cocoa by LC-MS/MS

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Abstract

This work proposes an extraction method based on the “dilute and shoot” approach and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) for the simultaneous determination of 42 mycotoxins (34 quantified and 8 qualitatively studied) in dried cocoa bean samples. The purpose of the developed methodology was the reduction of co-extractives from the matrix and an efficient extraction without a cleanup step, and subsequent analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). In order to obtain the best extraction conditions, gravimetric tests were performed and parameters that influenced the extraction efficiency were evaluated, such as the proportion of extraction phases, amount of salt, acidification, and extraction time. The performance of the developed method was evaluated to ensure its reliability. Considering the recovery range of 70–120% as an accuracy parameter, four of the mycotoxins under study (acetyl T-2, tenuazonic acid, wortmannin, and zearalenone) showed undesirable values at one of the levels evaluated. The repeatability of the method was assessed for 34 mycotoxins by the relative standard deviation (RSD%) of the responses, and all presented satisfactory values. The quantification limits ranged from 1.0 to 33.0 μg kg−1. Modification of the extraction methods made it possible to simultaneously analyze multiple mycotoxins, eliminating the need for the cleanup step, which led to analyte losses. The proposed methodology has a low cost, which makes it advantageous in routine analysis. It also has the potential for scope extension to cocoa-based foods, which are naturally exposed to a greater variety of mycotoxins.

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Acknowledgments

This work was carried out with the support of Coordenação de Aperfeiçoamento de Pessoal de Nível Superior – Brazil (CAPES) – Financing code 001. The authors also thank the Laboratório de Controle de Qualidade e Segurança Alimentar (LACQSA-BH), Laboratório Nacional Agropecuário de Minas Gerais (LANAGRO-MG) and Laboratório de Analítica e Eletroanalítica da Universidade Federal de Lavras (LAE-UFLA) by the assignment of the facilities and equipment for the accomplishment of this work.

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Authors and Affiliations

  1. Chemistry Department, Federal University of Lavras, Lavras, MG, 37200-000, Brazil

    Daiane Cássia Pereira Abreu, Elisangela Jaqueline Magalhães & Adelir Aparecida Saczk

  2. Laboratory of Quality Control and Food Safety, National Agricultural Laboratory of Minas Gerais, Belo Horizonte, MG, 30380-090, Brazil

    Fabiano Aurélio da Silva Oliveira, Eugenia Azevedo Vargas & Fernando Diniz Madureira

  3. Chemistry Department, Federal University of Minas Gerais, Belo Horizonte, MG, 31270-901, Brazil

    Lucas Pinto da Silva

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  1. Daiane Cássia Pereira Abreu
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Abreu, D.C.P., da Silva Oliveira, F.A., Vargas, E.A. et al. Methodology development based on “dilute and shoot” and QuEChERS for determination of multiple mycotoxins in cocoa by LC-MS/MS. Anal Bioanal Chem 412, 1757–1767 (2020). https://doi.org/10.1007/s00216-020-02390-5

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