Journal
FOOD ADDITIVES AND CONTAMINANTS PART A-CHEMISTRY ANALYSIS CONTROL EXPOSURE & RISK ASSESSMENT
Volume 29, Issue 4, Pages 497-507Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/19440049.2011.604044
Keywords
chromatography - LC/MS; method validation; regulations; veterinary drug residues; veterinary drug residues - antibiotics; milk
Funding
- National Council for Scientific and Technological Development (CNPq)
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This study presents the development and validation of a simple method for the detection and quantification of six beta-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 (CC alpha), detection capability (CC alpha), accuracy, inter-and intra-day repeatability of the method are reported.
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