Concurrent determination of four fluoroquinolones in catfish, shrimp, and salmon by liquid chromatography with fluorescence detection

A liquid chromatographic (LC) method with fluorescence detection was developed for concurrent determination of 4 fluoroquinolones: ciprofloxacin (CIPRO), enrofloxacin (ENRO), sarafloxacin (SARA), and difloxacin (DIFLX) in catfish, shrimp, and salmon. The procedure consists of extraction from fish ti...

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Bibliographic Details
Published in:Journal of AOAC International 2002-11, Vol.85 (6), p.1293-1301
Main Authors: ROYBAL, José E, WALKER, Calvin C, PFENNING, Allen P, TURNIPSEED, Sherri B, STOREY, Joseph M, GONZALES, Steve A, HURLBUT, Jeffrey A
Format: Article
Language:English
Subjects:
Animals
Anti-Infective Agents - analysis
Biological and medical sciences
Calibration
Catfishes - metabolism
Chromatography, Liquid
Fish and seafood industries
Fluoroquinolones
Food industries
Food toxicology
Fundamental and applied biological sciences. Psychology
Indicators and Reagents
Milk - chemistry
Muscle, Skeletal - chemistry
Penaeidae - chemistry
Quality Control
Reference Standards
Salmon - metabolism
Solutions
Spectrometry, Fluorescence
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Summary:A liquid chromatographic (LC) method with fluorescence detection was developed for concurrent determination of 4 fluoroquinolones: ciprofloxacin (CIPRO), enrofloxacin (ENRO), sarafloxacin (SARA), and difloxacin (DIFLX) in catfish, shrimp, and salmon. The procedure consists of extraction from fish tissue with acidified ethanol, isolation and retention on a cation exchange solid-phase extraction column, elution with basic methanol, and LC analysis with fluorescence detection. LC is performed by isocratic elution with acetonitrile-2% acetic acid (16 + 84) mobile phase, and a PLRP-S polymer column with fluorescence detection, excitation 278 nm and emission 450 nm. A target level of 20 ppb for each of the 4 fluoroquinolones has been established for this method. Fortified and incurred fish sample results are based on a 5-point standard curve calculation (10-160 ppb). Overall percent recoveries (% relative standard deviation) from fortified catfish were 78 (10), 80 (11), 70 (9.4), and 78 (10); from fortified shrimp, 69 (5.9), 85 (4.9), 79 (5.9), and 90 (4.5); and from fortified salmon, 56 (15), 93 (5.6), 61 (11), and 87 (5.0) for CIPRO, ENRO, SARA, and DIFLX, respectively. Data from the analysis of fluoroquinolone-incurred catfish, shrimp, and salmon are presented.
ISSN:1060-3271
1944-7922
DOI:10.1093/jaoac/85.6.1293