title: Determination of residues of oxolinic acid and flumequine in freeze-dried salmon muscle and skin by HPLC with fluorescence detection.
abstract: A procedure for the determination of residues of oxolinic acid (OA) and flumequine (FLU) in freeze-dried salmon muscle with attached skin, using reversed-phase high-performance liquid chromatography, is described. OA and FLU were extracted by a solid-liquid extraction procedure: after addition of hydrochloric acid, extraction used successively ethyl acetate, sodium hydroxide and chloroform. Liquid chromatography was performed on a 5 microm PuroSpher RP-18E cartridge using acetonitrile and 0.02 M aqueous orthophosphoric acid solution as mobile phase, with fluorescence detection. The performance of the method was established by spiking tissues with OA and FLU before the freeze-drying step. The method was linear over the concentration range 50-2000 ng/g freeze-dried tissue. Limits of detection and quantitation were 3.2 and 16 ng/g wet weight tissue respectively both for OA and FLU. Mean extraction recoveries of OA and FLU from freeze-dried tissue were 85.5 and 85.2% respectively. The method is suitable as a regulatory one for determination of residues of OA and FLU in freeze-dried salmon tissue.
authors.affiliation: Ecole Nationale Vétérinaire de Nantes, Unité Mixte de Recherche INRA-ENVN de Chimiothérapie Aquacole et Environnement, France. pouliquen@vet-nantes.fr
authors.forename: H
authors.initials: H
authors.lastname: Pouliquen
authors.forename: M L
authors.initials: ML
authors.lastname: Morvan
mesh_terms: D000818:Animals; D000890:Anti-Infective Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis*; D024841:Fluoroquinolones; D005506:Food Contamination / Q000032:analysis*; D005612:Freeze Drying; D008460:Meat / Q000032:analysis*; D009132:Muscles / Q000737:chemistry; D010093:Oxolinic Acid / Q000032:analysis*; D011807:Quinolizines / Q000032:analysis*; D012015:Reference Standards; D012474:Salmon; D012867:Skin / Q000737:chemistry
chemical_list: D000890:Anti-Infective Agents; D024841:Fluoroquinolones; D011807:Quinolizines; D010093:Oxolinic Acid; C012976:flumequine