Multiresidue determination of fluoroquinolones in poultry muscle and kidney according to the regulation 2002/657/EC. A systematic comparison of two different approaches: Liquid chromatography coupled to high-resolution mass spectrometry or tandem mass spectrometry.

Diego G Rocha, Flavio A Santos, Júlio César C da Silva, Rodinei Augusti, Adriana F Faria

Index: J. Chromatogr. A. 1379 , 83-91, (2015)

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Abstract

This work involved the optimization and validation of two methods according to the Commission Decision 2002/657/EC directives for determining fluoroquinolones residues in samples of poultry muscle and kidney: ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, nalidixic acid, norfloxacin, ofloxacin, oxolinic acid, pipemidic acid and sarafloxacin. The extraction procedure was based on a QuEChERS approach, whose optimization employed a Box-Behnken 3(3) factorial design. A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed for determining the twelve analytes using the multiple reaction monitoring mode (MRM). Accuracy, evaluated by recovery studies, varied from 88.8 to 112.2% for the selected levels with RSD values lower than 12.3%. The second validated method employed high resolution mass spectrometry (HRMS) performed in the single ion monitoring mode (SIM), determining nine among twelve analytes. The validation parameters were evaluated as satisfactory, with recoveries from 82.5 to 114.4% and RSD lower than 8.7%. Decision limits and detection capabilities for both methods were reported. The two methods were statistically compared using the Student's t test, at 95% confidence level, resulting in no significant difference. Copyright © 2015. Published by Elsevier B.V.