title: Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LC-ESI-MS/MS approach based on advanced mass spectrometric techniques.
abstract: A strategy was newly developed to rapidly screen seventeen sulfonamides and five tetracyclines in a single run from fish tissues using ultra-high performance liquid chromatography (UHPLC) coupled with comprehensive mass spectrometric approaches, including precursor-ion scan and data dependent scan. The product ions for precursor-ion scanning were selected by studying the MS/MS fragmentation of the analytes. All sulfonamides share the same diagnostic product ion at m/z 156 in positive MS/MS scan, while for tetracycline antibiotics the diagnostic product ion was proved to be at m/z 153.8. Further characterization of each compound was performed using a data dependent scan. Separation was performed on a Zorbax Eclipse Plus C18 column with a gradient elution using acetonitrile - 0.1% formic acid mobile phase at a flow rate of 0.1 mL min(-1). This approach has proven to be a powerful, highly selective, and sensitive tool for rapid screening and detection of non-targeted components in fish tissue and requires a minimum sample preparation such as one generic extraction step with MeOH:ACN 50:50 (v/v) acidified with 0.05% formic acid. The method has also been applied successfully to porcine and poultry meat. The validation of such a screening method was performed for the first time according to Commission Decision 2002/657/EC and satisfactory method performance characteristics were achieved.
authors.affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis Zographou, 15771 Athens, Greece.
authors.forename: Marilena E
authors.initials: ME
authors.lastname: Dasenaki
authors.forename: Nikolaos S
authors.initials: NS
authors.lastname: Thomaidis
mesh_terms: D053000:Analytic Sample Preparation Methods; D000818:Animals; D002645:Chickens; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005396:Fish Products / Q000032:analysis*; D005399:Fishes; D008460:Meat / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013449:Sulfonamides / Q000032:analysis*; D013552:Swine; D013754:Tetracyclines / Q000032:analysis*
chemical_list: D013449:Sulfonamides; D013754:Tetracyclines