title: Rapid method for the determination and confirmation of fluoroquinolone residues in catfish using liquid chromatography/fluorescence detection and liquid chromatography-tandem mass spectrometry.
abstract: A simplified method for the extraction and determination of four fluoroquinolone (FQ) residues (ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) in catfish is presented. In this method, the FQ residues were extracted with acidified acetonitrile, and the extract was defatted with dispersive C18 solid-phase extraction (SPE) sorbent or hexane. A portion of the extract was evaporated and reconstituted in the mobile phase. The quantitative determination was accomplished with LC-fluorescence detection (FLD), and the confirmation was by LC-MS/MS. Fortifications of catfish tissue were carried out at 0.5x, x, 2x, and 4x, where x = 5 ppb (U.S. Food and Drug Administration current regulatory target level). Recoveries for the LC/FLD determination of five replicates (for both cleanup routes) at each level ranged from 64 to 98%, with RSD values <8%. The method quantitation limits for all residues were <1 ng/g. The LC-MS/MS analysis of the same extracts confirmed all FQ residues at all levels. This method is an improvement over existing methodologies since additional cleanup steps, such as cation exchange SPE column cleanup, are not utilized. The C18 dispersive SPE method represents a novel cleanup approach for FQs in fish tissue.
authors.affiliation: U.S. Food and Drug Administration, Southeast Regional Laboratory, 60 Eighth St NE, Atlanta, GA 30309, USA. sarah.mcmullen@fda.hhs.gov
authors.forename: Sarah E
authors.initials: SE
authors.lastname: McMullen
authors.forename: Frank J
authors.initials: FJ
authors.lastname: Schenck
authors.forename: Victor A
authors.initials: VA
authors.lastname: Vega
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002397:Catfishes / Q000378:metabolism*; D002851:Chromatography, High Pressure Liquid; D004350:Drug Residues / Q000032:analysis*; D024841:Fluoroquinolones / Q000032:analysis*; D006586:Hexanes; D007202:Indicators and Reagents; D012015:Reference Standards; D052616:Solid Phase Extraction; D012996:Solutions; D012997:Solvents; D013050:Spectrometry, Fluorescence; D053719:Tandem Mass Spectrometry
chemical_list: D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D006586:Hexanes; D007202:Indicators and Reagents; D012996:Solutions; D012997:Solvents