Multi-residue determination of antibiotics in fish by liquid chromatography-tandem mass spectrometry

• Published in: Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment Chemistry, analysis, control, exposure & risk assessment, 2013-06, Vol.30 (6), p.940-948
• Main Authors: Gbylik, M, Posyniak, A, Mitrowska, K, Bladek, T, Zmudzki, J
• Format: Article
• Language: English
• Subjects: acetonitrile; aminoglycosides; Animals; Anti-Bacterial Agents - analysis; Antibiotics; beta-lactams; Biological and medical sciences; Chemical compounds; Chromatography; Drug Residues - analysis; Fish; Fish and seafood industries; Fishes; fluoroquinolones; Food industries; Fundamental and applied biological sciences. Psychology; Laboratories; LC-MS/MS; Limit of Detection; macrolides; Mass spectrometry; multi-residue; multiresidue analysis; Reproducibility of Results; sulfonamides; Tandem Mass Spectrometry - methods; tetracyclines; trimethoprim
• ISSN: 1944-0057; 1944-0049; 1944-0057
• DOI: 10.1080/19440049.2013.780210

A multi-residue method for the determination of 34 antibacterial drugs (three aminoglycosides, nine β-lactams, nine fluoroquinolones, three macrolides, five sulfonamides, trimethoprim and four tetracyclines) in fish samples by LC-MS/MS was developed. The procedure enables the isolation of residues based on double extraction of the fish sample with m-phosphoric acid and heptafluorobutyric acid as an ion-pair agent and acetonitrile. All compounds were determined at the same time on a C18 column with gradient elution. The method was validated according to the requirements of European Decision 2002/657/EC. Specificity, recovery, repeatability, within-laboratory reproducibility, decision limit CCα and detection capability CCβ were calculated. CCα ranged from 55.3 to 1085 µg kg⁻¹ and CCβ ranged from 59.5 to 1141 µg kg⁻¹. The overall recoveries were from 96% to 111% with respect to the internal standards.