Determination of oxolinic acid residues in salmon muscle tissue by liquid chromatography with fluorescence detection

• Published in: Journal of the Association of Official Analytical Chemists Vol. 74; no. 4; p. 608
• Main Authors: Larocque, L. (Health and Welfare Canada, Ottawa, Ontario, Canada), Schnurr, M, Sved, S, Weninger, A
• Format: Journal Article
• Language: English
• Published: United States 01.07.1991
• Subjects: ACIDE OXALIQUE; ACIDO OXALICO; ALIMENT POUR ANIMAUX; ANIMAL PHYSIOLOGY; Animals; Calibration; CHROMATOGRAPHIE; CHROMATOGRAPHY; Chromatography, Liquid - methods; CROMATOGRAFIA; Drug Residues - analysis; Drug Residues - pharmacokinetics; DRUGS; EXTRACTION; FEEDS; FISIOLOGIA ANIMAL; Fluorescence; Fluorometry - methods; MEDICAMENT; MEDICAMENTOS; Microchemistry - methods; MUSCLE; MUSCLES; Muscles - chemistry; Muscles - metabolism; MUSCULOS; OPTICAL PROPERTIES; OXALIC ACID; Oxolinic Acid - analysis; Oxolinic Acid - pharmacokinetics; PHYSIOLOGIE ANIMALE; PIENSOS; PROPIEDADES OPTICAS; PROPRIETE OPTIQUE; RESIDU; RESIDUES; RESIDUOS; SALMON; Salmon - metabolism; SAUMON
• ISSN: 0004-5756
• DOI: 10.1093/jaoac/74.4.608

The present paper describes a method for determination of oxolinic acid in salmon muscle tissue. Tissue (0.5-2 g) mixed with 2 g anhydrous sodium sulfate is extracted twice with ethyl acetate, centrifuged, and the extract evaporated. The residue is partitioned in a mixture of hexane and 0.01M oxalic acid and the aqueous phase chromatographed using fluorescence detection at 327 nm excitation and 369 nm emission. Calibration and standard curves are linear from 10-200 ppb and 100-2000 ppb at different sensitivity settings. Recoveries ranged from 71-83% in spiked blanks, with a CV of 4-10.3% over a 2-week period. Preliminary results in treated salmon were variable, possibly because some fish refused to eat medicated feed.