title: β-lactam antibiotics residues analysis in bovine milk by LC-ESI-MS/MS: a simple and fast liquid-liquid extraction method.
abstract: 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 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 (CCβ), accuracy, inter- and intra-day repeatability of the method are reported.
authors: Laboratório Nacional Agropecuário - Lanagro/RS, Porto Alegre, RS, Brazil. louisejank@gmail.com
authors: L
authors: L
authors: Jank
authors: R B
authors: RB
authors: Hoff
authors: P C
authors: PC
authors: Tarouco
authors: F
authors: F
authors: Barreto
authors: T M
authors: TM
authors: Pizzolato
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001938:Brazil; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D019155:Veterinary Drugs / Q000032:analysis; D047090:beta-Lactams / Q000032:analysis*
chemical_list: D000900:Anti-Bacterial Agents; D019155:Veterinary Drugs; D047090:beta-Lactams