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Validation of a method for the analysis of quinolones residues in bovine muscle by liquid chromatography with electrospray ionisation tandem mass spectrometry detection
Authors:A Rubies  F Centrich  M Granados
Institution:a Laboratori Agència Salut Pública de Barcelona, Avda. de les Drassanes 13-15, E-08001 Barcelona, Spain
b Departament de Química Analítica, Universitat de Barcelona, Martí i Franquès 1-11, E-08028 Barcelona, Spain
Abstract:A liquid chromatography-tandem mass spectrometry method for the determination and confirmation of nine quinolones was optimised and validated according to Commission Decision 2002/657/EC. Analytes were extracted from veal muscle with water and extracts purified with 96-well plates Oasis HLB cartridges. Separation was carried out in a silica-based C18 column (50 mm × 2.1 mm) with mobile phases consisting of water/acetonitrile mixtures containing acetic acid. Linear calibration curves in the ranges 4-400 and 50-800 ng g−1, with correlation coefficients at least 0.995, were obtained for all the analytes. At concentration levels above 10 ng g−1, quantification errors were lower than 10% and repeatability and within-laboratory reproducibility standard deviations below 6% and 10%, respectively. Decision limits and detection capabilities are reported.
Keywords:Quinolones  Residue analysis  Bovine muscle  Liquid chromatography  Tandem mass spectrometry
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