This paper presents an analytical method for the determination of quinolones in chicken tissues. The procedure involves pre-treatment by solid-phase extraction (SPE) and subsequent liquid chromatography (LC) with UV absorbance detection. Different SPE disposable cartridges and extractants of the tissue samples were tested, and various columns were systematically tested. The mobile phase was composed of acetonitrile and citric buffer at pH 4.5, with an initial composition of acetonitrile-water (12:88, v/v) and using linear gradient elution. Recoveries were 66-91% in the concentration range 30-300 microg kg(-1). The detector response was linear in this range. The limits of detection were 16-30 microg kg(-1). These values were lower than the maximum residue limits established by the European Union.
"In previous studies, analyses of quinolones from food samples by LC-UV were performed with 10 mM citric acid with different percentages of MeCN at pH 4.5 using a gradient elution timetable (Garcés et al., 2006; Hermo et al., 2006; Bailac et al., 2004). When the biological sample is cow or pig plasma, the pH of the mobile phase should to be changed to pH 5.0 in order to obtain better resolution between peaks of SAR and DIF. "
[Show abstract][Hide abstract] ABSTRACT: This paper presents the multiresidue determination of the series of quinolones regulated by the European Union (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid and flumequine) in bovine and porcine plasma using capillary electrophoresis and liquid chromatography with ultraviolet detection (CE-UV, LC-UV), liquid chromatography-mass spectrometry and -tandem mass spectrometry (LC-MS, LC-MS/MS) methods. These procedures involve a sample preparation by solid-phase extraction for clean-up and preconcentration of the analytes before their injection into the separation system. All methods give satisfactory results in terms of linearity, precision, accuracy and limits of quantification. The suitability of the methods to determine quinolones was evaluated by determining the concentration of enrofloxacin and ciprofloxacin in real samples from pig plasma and cow plasma.
[Show abstract][Hide abstract] ABSTRACT: We have developed a heterologous direct competitive enzyme-linked immunosorbent assay (ELISA) and a visual colloidal gold-based
immunochromatographic assay (CGIA) for simultaneous determination of ofloxacin, marbofloxacin, and fleroxacin residues in
milk using polyclonal antibodies. The half-maximum inhibition concentrations (IC50) of ofloxacin, marbofloxacin, fleroxacin, and limits of detection (LODs; calculated as IC15 values) are between 0.20 and 0.53ng mL−1, and between 0.02 and 0.05ng mL−1, respectively. The average recoveries range from of 78% to 113%, and the coefficients of variation of intra- and inter-assays
are between 2 and 11%, and 3 to 19%, respectively. The LODs for ofloxacin, marbofloxacin, fleroxacin in milk are between 3.5
and 8.9ng mL−1. The visual minimum detection limit of the optimized CGIA is 2ng mL−1 for milk samples. The detection process can be completed within 10min. The strips can be stored at 4°C for 8weeks without
significant loss of activity. The results of the analysis of spiked samples showed that the CGIA can be applied to preliminary,
fast, and on-site screening of milk samples. The ELISA and CGIA allow for a rapid, sensitive, and low-cost determination of
(fluoro)quinolones residues in milk samples.
FigureA direct competitive enzyme-linked immunosorbent assay (ELISA) and a visual colloidal gold-based immunochromatographic assay
(CGIA) are proposed for simultaneous determination of ofloxacin, marbofloxacin, and fleroxacin residues in milk using polyclonal
[Show abstract][Hide abstract] ABSTRACT: This work presents a comparison between three analytical methods developed for the simultaneous determination of eight quinolones regulated by the European Union (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, difloxacin, sarafloxacin, oxolinic acid and flumequine) in pig muscle, using liquid chromatography with fluorescence detection (LC–FD), liquid chromatography–mass spectrometry (LC–MS) and liquid chromatography-tandem mass spectrometry (LC–MS/MS). The procedures involve an extraction of the quinolones from the tissues, a step for clean–up and preconcentration of the analytes by solid-phase extraction and a subsequent liquid chromatographic analysis. The limits of detection of the methods ranged from 0.1 to 2.1 ng g−1 using LC–FD, from 0.3 to 1.8 using LC–MS and from 0.2 to 0.3 using LC–MS/MS, while inter- and intra-day variability was under 15 % in all cases. Most of those data are notably lower than the maximum residue limits established by the European Union for quinolones in pig tissues. The methods have been applied for the determination of quinolones in six different commercial pig muscle samples purchased in different supermarkets located in the city of Granada (south-east Spain).
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