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Development and Validation of a Multiclass Method for the Analysis of Veterinary Drug Residues in Eggs Using Liquid Chromatography-Tandem Mass Spectrometry

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Abstract

A liquid chromatography tandem-mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of 22 veterinary drug residues, belonging to eight classes (coccidiostats, lincosamides, macrolides, tetracyclines, sulfonamides, benzimidazoles, diterpenes, and diaminopyrimidines), in eggs. Chromatographic separations were achieved on an XBridge BEH C18 column (150 × 2.1 mm, 3.5 μm, Waters, USA) maintained at 35 °C. The mobile phase was eluted at 400 μL min−1 in gradient mode between water and methanol/acetonitrile (20:80 v/v), both containing 0.1 % formic acid. The samples were prepared by protein precipitation with acetonitrile without additional cleanup steps. The method was successfully validated according to the Commission Decision 2002/657/EC and was demonstrated to be highly selective and free of matrix and residual effects. The method presented low limits of detection (0.37 to 7.5 μg kg−1) and quantification (1.25 to 20 μg kg−1). For banned substances, the decision limit values (CCα) and detection capability (CCβ) were 0.62–7.5 and 0.65–8.1 μg kg−1, respectively. For substances with a maximum residue limit, the CCα and CCβ values were 2.15–1061.5 and 2.3–1135.9 μg kg−1, respectively. All calibration curves showed excellent correlation (r ≥ 0.99). The recovery of the analytes and internal standards (49.0–103.7 %) was reached with high precision (RSD <8 %). At different concentration levels, the variations in precision and accuracy, in terms of repeatability and in-laboratory reproducibility, were <11 %. The new method is applicable to the routine analysis of commercial egg samples.

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Acknowledgments

The authors would like to thank the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) for the scholarship, and Fundação Araucária for the financial support.

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Authors and Affiliations

  1. Departamento de Farmácia, Universidade Federal do Paraná, 632 Lothário Meissner Avenue, Curitiba, Paraná, 80210-170, Brazil

    Flávia Lada Degaut Pontes, João Cleverson Gasparetto, Thais Martins Guimarães de Francisco, Heloise Calzado Goetzke, Letícia Paula Leonart & Roberto Pontarolo

  2. Laboratório Central do Estado do Paraná, Curitiba, Paraná, Brazil

    Daniel Altino de Jesus

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  1. Flávia Lada Degaut Pontes
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  2. João Cleverson Gasparetto
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  5. Letícia Paula Leonart
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Correspondence to Roberto Pontarolo.

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Conflict of Interest

Flávia Lada Degaut Pontes declares that she has no conflict of interest. João Cleverson Gasparetto declares that he has no conflict of interest. Thais Martins Guimarães de Francisco declares that she has no conflict of interest. Heloise Calzado Goetzke declares that she has no conflict of interest. Letícia Paula Leonart declares that she has no conflict of interest. Daniel Altino de Jesus declares that he has no conflict of interest. Roberto Pontarolo declares that he has no conflict of interest.

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Pontes, F.L.D., Gasparetto, J.C., de Francisco, T.M.G. et al. Development and Validation of a Multiclass Method for the Analysis of Veterinary Drug Residues in Eggs Using Liquid Chromatography-Tandem Mass Spectrometry. Food Anal. Methods 10, 1063–1077 (2017). https://doi.org/10.1007/s12161-016-0670-8

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