University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Website: @unf

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Classification: Marine -> fish -> catfish

Citations 1

"Determination Of Residues Of Flumequine And Nalidixic, Oxolinic, And Piromidic Acids In Catfish By Liquid Chromatography With Fluorescence And UV Detection"
J. AOAC Int. 1995 Volume 78, Issue 2 Pages 343-352
Robert K. Munns, Sherri B. Turnipseed, Allen P. Pfenning, José E. Roybal, David C. Holland, Austin R. Long, and Steven M. Plakas

Abstract: A liquid-chromatographic (LC) method is described for determining residues of flumequine (FLU) and nalidixic (NAL), oxolinic (OXO), and piromidic (PIR) acids in catfish muscle. The identities of 3 of these residues are confirmed by gas chromatography-mass spectrometry (GC-MS). The extraction and cleanup procedures are the same for both determination and identification. Analyte isolation involves homogenizing the tissue with acetone, defatting the acetone extract with hexane, and extracting the compounds into chloroform. The extract is further purified by first partitioning into base and subsequently back-extracting into chloroform after acidifying the aqueous phase. After the solvent is evaporated, the residue is dissolved in mobile phase, and the analytes are determined by LC with fluorescence detection, excitation at 325 nm and emission at 365 nm. Catfish muscle was fortified with each quinolone at 5, 10, 20, 40, and 80 ng/g. Recoveries were 83-94%, with relative standard deviations (RSDs) of 5-7%. The method was evaluated also by a second analyst, who determined 4 quinolones added in combination. Average recoveries of quinolones from catfish fortified at 5, 10, and 20 ng/g were 78-90%, with RSDs of 3-6%. The presence in catfish muscle of incurred OXO, FLU, and NAL at the 10 ng/g level was confirmed by analyzing the decarboxylated quinolones by GC-MS. The relative abundances of all 5 major ions for OXO, FLU, and NAL were within 10% of those observed in spectra of standard compounds decarboxylated by the same method.
Flumequine Nalidixic acid Oxolinic acid Piromidic acid LC Fluorescence Spectrophotometry Post-column derivatization