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β-lactam antibiotics residues analysis in bovine milk by LC-ESI-MS/MS: a simple and fast liquid–liquid extraction method

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This study presents the development and validation of a simple method for the detection and quantification of six β-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 C18 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 (CCβ), accuracy, inter- and intra-day repeatability of the method are reported.
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Keywords: chromatography – LC/MS; method validation; milk; regulations; veterinary drug residues; veterinary drug residues – antibiotics

Document Type: Research Article

Affiliations: 1: Laboratório Nacional Agropecuário – Lanagro/RS,Porto Alegre, RS, Brazil 2: Instituto de Química, Universidade Federal do Rio Grande do Sul – UFRGS, Porto Alegre,RS, Brazil

Publication date: April 1, 2012

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