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Determination of amoxicillin in catfish and salmon tissues by liquid chromatography with precolumn formaldehyde
1National Center for Toxicological Research, U.S. Food and Drug Administration, Jefferson, AR 72079-9502, USA.
Abstract:
A liquid chromatographic (LC) method with fluorescence detection was developed for analysis of amoxicillin in catfish and salmon tissues. The tissue was extracted with phosphate buffer (pH 4.5), followed by trichloroacetic acid (TCA) precipitation of proteins and solid-phase (C18) extraction. Trace amounts of nonpolar interfering substances present after solid-phase extraction were removed by ether liquid-liquid extraction. The extract was reacted with formaldehyde and TCA at 100 degrees C for 30 min. A fluorescent derivative was extracted with ether, concentrated, and analyzed by reversed-phase LC with fluorescence detection. Average recoveries of amoxicillin spiked at 2.5-20 ppb were > 80% for catfish and > 75% for salmon muscle tissue, with coefficients of variation of < 6%. Limits of detection (LOD) and quantitation (LOQ) for catfish tissue were 0.5 and 1.2 ppb, respectively. LOD and LOQ for salmon muscle tissue were 0.8 and 2.0 ppb, respectively.