Phenylboronic Acid Solid Phase Extraction Cleanup and Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Florfenicol Amine in Fish Muscles.

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Sin DW, Ho C, Wong YT

Phenylboronic Acid Solid Phase Extraction Cleanup and Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Florfenicol Amine in Fish Muscles.

J AOAC Int. 2015 May-Jun;98(3):566-74. doi: 10.5740/jaoacint.14-267. Epub 2015 May 28.

PubMed ID
26025252 [ View in PubMed
]
Abstract

Florfenicol (FFC) residues in foods are regulated as the sum of florfenicol and its metabolites measured as florfenicol amine (FFA). An isotope dilution LC-MS/MS method utilizing phenylboronic acid (PBA) SPE cleanup is established for the accurate determination of FFA in fish muscles (i.e., salmon and tilapia) after acid catalyzed hydrolysis. Comparisons of the PBA SPE cleanup procedure with other cleanup procedures such as mixed-mode cationic (MCX) SPE and solid supported liquid-liquid extraction were performed. Quantification of FFA in fish muscles was accomplished by using matrix-matched calibration with FFA-D3 as the internal standard. The method was validated with FFA fortified fish muscles at three different levels (50, 100, and 200 mug/kg). Conversion of FFC to FFA by acid catalyzed hydrolysis was evaluated and found to be >/=88%. The recoveries of FFA in fish muscles at the three fortification levels ranged from 89 to 106%, and RSDs were

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