title: High-throughput method for the determination of residues of β-lactam antibiotics in bovine milk by LC-MS/MS.
abstract: This study describes the development and validation procedures for scope extension of a method for the determination of β-lactam antibiotic residues (ampicillin, amoxicillin, penicillin G, penicillin V, oxacillin, cloxacillin, dicloxacillin, nafcillin, ceftiofur, cefquinome, cefoperazone, cephapirine, cefalexin and cephalonium) in bovine milk. Sample preparation was performed by liquid-liquid extraction (LLE) followed by two clean-up steps, including low temperature purification (LTP) and a solid phase dispersion clean-up. Extracts were analysed using a liquid chromatography-electrospray-tandem mass spectrometry system (LC-ESI-MS/MS). Chromatographic separation was performed in a C18 column, using methanol 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. Main validation parameters such as linearity, limit of detection, decision limit (CCα), detection capability (CCβ), accuracy, and repeatability were determined and were shown to be adequate. The method was applied to real samples (more than 250) and two milk samples had levels above maximum residues limits (MRLs) for cloxacillin - CLX and cefapirin - CFAP.
authors.affiliation: a Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.|b Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , Brazil.
authors.forename: Louise
authors.initials: L
authors.lastname: Jank
authors.affiliation: b Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , Brazil.|c Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.
authors.forename: Magda Targa
authors.initials: MT
authors.lastname: Martins
authors.affiliation: a Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.|b Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , Brazil.
authors.forename: Juliana Bazzan
authors.initials: JB
authors.lastname: Arsand
authors.affiliation: a Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.|b Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , Brazil.
authors.forename: Rodrigo Barcellos
authors.initials: RB
authors.lastname: Hoff
authors.affiliation: b Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , Brazil.|c Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.
authors.forename: Fabiano
authors.initials: F
authors.lastname: Barreto
authors.affiliation: a Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.
authors.forename: Tânia Mara
authors.initials: TM
authors.lastname: Pizzolato
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000737:chemistry / Q000302:isolation & purification*; D002511:Cephalosporins / Q000737:chemistry / Q000302:isolation & purification*; D002853:Chromatography, Liquid; D004350:Drug Residues / Q000737:chemistry / Q000302:isolation & purification*; D005506:Food Contamination / Q000032:analysis; D005561:Formates; D006801:Humans; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction; D000432:Methanol; D008892:Milk / Q000737:chemistry*; D010406:Penicillins / Q000737:chemistry / Q000302:isolation & purification*; D015203:Reproducibility of Results; D012997:Solvents; D021241:Spectrometry, Mass, Electrospray Ionization; D014867:Water
chemical_list: D000900:Anti-Bacterial Agents; D002511:Cephalosporins; D005561:Formates; D010406:Penicillins; D012997:Solvents; D014867:Water; C030544:formic acid; D000432:Methanol
keywords: antibiotics residues; bovine milk; cephalosporins; mass spectrometry; penicillins