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Multi-residue and multi-class method for the determination of antibiotics in bovine muscle by ultra-high-performance liquid chromatography tandem mass spectrometry
Authors:Andreia Freitas  Jorge Barbosa  Fernando Ramos
Affiliation:1. INIAV-LNIV, Laboratório Nacional de Investigação Veterinária, Estrada de Benfica, 701, 1549-011 Lisboa, Portugal;2. CNC — Centro de Neurociências e Biologia Celular, Pólo das Ciências da Saúde, Faculdade de Farmácia, Universidade de Coimbra, Azinhaga de Santa Comba, 3000-548 Coimbra, Portugal
Abstract:A multi-residue quantitative screening method covering 41 antibiotics from 7 different families, by ultra-high-performance–liquid-chromatography tandem mass spectrometry (UHPLC–MS/MS), is described. Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol are simultaneously detected after a simple sample preparation of bovine muscle optimized to achieve the best recovery for all compounds. A simple sample treatment was developed consisting in an extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA), followed by a defatting step with n-hexane. The methodology was validated, in accordance with Decision 2002/657/EC by evaluating the required parameters: decision limit (CCα), detection capability (CCβ), specificity, repeatability and reproducibility. Precision in terms of relative standard deviation was under 20% for all compounds and the recoveries between 91% and 119%. CCα and CCβ were determined according the maximum residue limit (MRL) or the minimum required performance limit (MRPL), when required.
Keywords:Antibiotics   Multi-class   Multi-detection   UHPLC&ndash  MS/MS   Muscle   Validation
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