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A terbium-sensitized luminescence method is described for the determination of the sum of residues of enrofloxacin and its major metabolite ciprofloxacin in edible animal tissues. Several parameters affecting both detection and extraction were studied. Analytes were extracted from spiked samples of chicken and trout tissues with pH 7.4 buffer-dichloromethane. The organic extract was evaporated and the residue dissolved in aqueous nitric acid and defatted with hexane. Determination was carried out directly in the aqueous phase (in a micellar medium). The calibration curves were linear up to 75 micrograms l-1. The detection limit was 3.5 micrograms kg-1 (for a 5 g sample) and the repeatability was 7.0% (n = 7). The sensitivity was similar for both quinolones and therefore calibration can be carried out with either ciprofloxacin or enrofloxacin. In any case, the differences were < 10%.

A new screening method for the analysis of enrofloxacin and ciprofloxacin in edible animal tissues is described. The method is based on the application of principal component regression to luminescence measurements after reaction of quinolones with terbium(III) in a micellar medium. The method was used, first, to discriminate between quinolone-containing or quinolone-not-containing samples (concentration below the detection limit) and, then, to quantify the sum of both analytes. Standards in a pure-water matrix, using the first three principal components, were used for the determination. RRMSE range from 4 to 10% depending on the analyte. Calibration was successfully applied to the analysis of spiked chicken and trout muscle at concentrations between 10 and 50 micrograms kg-1.

SummaryA liquid chromatographic method has been developed to separate a series of quinolones which are wiclely used as veterinary drugs: clanofloxacin, clifloxacin, enrofloxacin (and its metabolite ciprofloxacin), marbofloxacin, norfloxacin and sarafloxacin. Separation was performed by using an end-capped high-purily silica-based C8 column and a mobile phase consisting of acetonitrile-aqueous oxalic acid buffer solution. In order to establish the optimal conditions for an isocratic separation, a three-factor Doehlert experimental design was applied. Gradient elution was applied which reduced analysis time. Figures of merit of the method proposed, with fluorimetric detection, were evaluated.

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SummaryThe dissociation constants of several quinolones in a 7 % acetonitrite-water mixture are determined. A model describing the effect of pH on the retention of quinolones by an octadecylsilica stationary phase with a 7 % acetonitrile-water mobile phase is proposed. The model uses pH values in the mobile phase instead of pH values in water and takes into account the effect of activity coefficients. Fluorescence of quinolones in the mobile phase is studied, and a chromatographic separation with fluorimetric detection is established. Detection limits for the proposed method range from 3 to 12 gg.L q.

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