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Article in English | MEDLINE | ID: mdl-21988179

ABSTRACT

This study presents the development and validation of a simple method for the detection and quantification of six ß-lactam antibiotics residues (ceftiofur, penicillin G, penicillin V, oxacillin, cloxacillin and dicloxacillin) in bovine milk using a fast liquid-liquid extraction (LLE) for sample preparation, followed by liquid chromatography-electrospray-tandem mass spectrometry (LC-MS/MS). LLE consisted of the addition of acetonitrile to the sample, followed by addition of sodium chloride, centrifugation and direct injection of an aliquot into the LC-MS/MS system. Separation was performed in a C(18) column, using acetonitrile and water, both with 0.1% of formic acid, as mobile phase. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Limits of detection ranged from 0.4 (penicillin G and penicillin V) to 10.0 ng ml(-1) (ceftiofur), and linearity was achieved. The decision limit (CCα), detection capability (CCß), accuracy, inter- and intra-day repeatability of the method are reported.


Subject(s)
Anti-Bacterial Agents/analysis , Drug Residues/analysis , Food Contamination/analysis , Liquid-Liquid Extraction/methods , Milk/chemistry , beta-Lactams/analysis , Animals , Brazil , Cattle , Chromatography, Liquid/methods , Limit of Detection , Reproducibility of Results , Spectrometry, Mass, Electrospray Ionization/methods , Tandem Mass Spectrometry/methods , Veterinary Drugs/analysis
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