Determination of florfenicol in fish feed by liquid chromatography.
A simple, accurate, and reproducible assay was developed for the determination of Florfenicol in medicated fish feed. Florfenicol was extracted from ground feed into an acetonitrile-water mixture by shaking and sonication. A portion of the centrifuged extract was passed through an Envi-Carb solid-phase extraction cartridge, through which Florfenicol eluted unretained. The collected eluant was diluted to adjust for analyte concentration, and injected into a reversed-phase liquid chromatography system. Samples were quantitated by external standard analysis versus multilevel calibration solutions. The procedure is suitable for the quantitation of samples medicated with 0.2-4 g/kg Florfenicol. Accuracy was evaluated by 2 analysts, who determined recovery of Florfenicol from feeds fortified over a range of 0.1-6.0 g/kg. The average recovery was 100.5% (relative standard deviation, 1.2%). The linearity, accuracy, precision, reproducibility (interday and analyst), and selectivity of the method are presented. The detection and quantitation limits were determined to be 0.2 and 1.0 mg/kg, respectively.
Hayes
John M
JM
Schering-Plough Research Institute, Analytical Development, 2000 Galloping Hill Rd, Kenilworth, NJ 07033, USA. john.hayes@spcorp.com
D000821:Animal Feed; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis; D002138:Calibration; D002498:Centrifugation; D002845:Chromatography; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis; D005223:Fats; D005399:Fishes; D005506:Food Contamination; D006863:Hydrogen-Ion Concentration; D009821:Oils; D012015:Reference Standards; D012044:Regression Analysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents; D013839:Thiamphenicol / Q000031:analogs & derivatives* / Q000032:analysis
D000900:Anti-Bacterial Agents; D005223:Fats; D009821:Oils; D012997:Solvents; C035534:florfenicol; D013839:Thiamphenicol