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A LC-HRMS After QuEChERS Cleanup Method for the Rapid Determination of Dye Residues in Fish Products

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Abstract

The reliability of a rapid LC-HRMS method was studied in order to find a sensitive and accurate, simple, cheap, and rapid method for screening and quantitative determination of malachite green (MG), leucomalachite green (LMG), brilliant green (BG), crystal violet (CV), and leucocrystal violet (LCV) in fish muscle. All the analytes were extracted using a mixture of acetonitrile and citrate buffer, while the cleanup phase was carried out by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. All the data analyzed were acquired using both full MS and dd-MS2 modes. Good specificity, precision (relative standard deviation <11% for each sample tested), recovery (10–60%), decision limit (CCα between 0.55 and 0.62 μg kg−1), detection capabilities (CCβ between 0.65 and 0.78 μg kg−1), and ruggedness were achieved for the reliability of the method. Satisfactory results were obtained during the linearity test in the range of 0.10–2 ng mL−1 (r 2 > 0.999). Best recoveries were obtained by the QuEChERS cleanup method for all the analytes examined, presenting values between 70 and 104%. The application of 70,000 FWHM mass resolution and narrow mass windows significantly improved the selectivity of the method, leading to simultaneous screening and quantification of dye residues in comparison to other methods proposed in literature. The optimized method proposed in this work enables a simple and fast preparation; it offers exceptional sensitivity and selectivity and maximizes efficiency and reproducibility with a low consumption of reagents. Finally, the present method was successfully employed to detect dye residues in 73 fish samples, as provided for the national residue control plan.

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Authors and Affiliations

  1. Istituto Zooprofilattico Sperimentale della Sicilia “A. Mirri”, Via Gino Marinuzzi, 3, 90129, Palermo, Italy

    Vita Giaccone, Gaetano Cammilleri, Andrea Macaluso, Antonio Vella & Vincenzo Ferrantelli

  2. Dipartimento Biomorf, Pan Lab, Università di Messina, V.le Annunziata, Messina, Italy

    Nicola Cicero

  3. Dipartimento di Scienze della Vita, Università degli studi di Modena e Reggio Emilia, Via Università 4, 41121, Modena, Italy

    Andrea Pulvirenti

Authors
  1. Vita Giaccone
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  2. Gaetano Cammilleri
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  3. Andrea Macaluso
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  4. Nicola Cicero
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  5. Andrea Pulvirenti
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  6. Antonio Vella
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  7. Vincenzo Ferrantelli
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Correspondence to Gaetano Cammilleri.

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Vita Giaccone declares that she has no conflict of interest. Gaetano Cammilleri declares that he has no conflict of interest. Andrea Macaluso declares that she has no conflict of interest. Nicola Cicero declares that she has no conflict of interest. Andrea Pulvirenti declares that she has no conflict of interest. Antonio Vella declares that he has no conflict of interest. Vincenzo Ferrantelli 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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Giaccone, V., Cammilleri, G., Macaluso, A. et al. A LC-HRMS After QuEChERS Cleanup Method for the Rapid Determination of Dye Residues in Fish Products. Food Anal. Methods 11, 625–634 (2018). https://doi.org/10.1007/s12161-017-1032-x

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  • DOI: https://doi.org/10.1007/s12161-017-1032-x

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