ABSTRACT
Most methods reported in the literature for determination of nitrofuran metabolites use the same extraction and derivatisation conditions to hydrolyse and extract the protein-bound residues from animal tissue. While undertaking certification of reference materials for nitrofuran metabolites in freeze-dried prawn, it was found that these conditions are satisfactory for recovery of spiked residues; however, extraction efficiencies of incurred furazolidinone could be substantially increased by further optimisation of the extraction conditions. The availability of a suitable certified reference material allows laboratories to ensure that their method is optimised for incurred residues.
Subject(s)
Crustacea/chemistry , Drug Residues/isolation & purification , Nitrofurans/isolation & purification , Animals , Chromatography, Liquid , Drug Residues/analysis , Nitrofurans/analysis , Tandem Mass SpectrometryABSTRACT
A reversed-phase high-performance liquid chromatographic method with tandem mass-spectrometric detection was developed and validated for the simultaneous analysis of eight quinolones and fluoroquinolones (oxolinic acid, flumequine, piromidic acid, enrofloxacin, ciprofloxacin, danofloxacin, sarafloxacin and orbifloxacin) in trout tissue, prawns and abalone. The analytes were extracted from homogenised tissue using acetonitrile and the extracts subjected to an automated two-stage solid-phase extraction process involving polymeric reversed-phase and anion-exchange cartridges. Good recoveries were obtained for all analytes and the limit of quantification was 5 microg/kg (10 microg/kg for ciprofloxacin). The limit of detection was 1-3 microg/kg, depending on the analyte and matrix. Confirmation of the identity of a residue was achieved by further tandem mass-spectrometric analysis. A procedure for estimating the uncertainty associated with the measurement is presented.
