Use of micellar liquid chromatography to analyze oxolinic acid, flumequine, marbofloxacin and enrofloxacin in honey and validation according to the 2002/657/EC decision

Abstract

A micellar liquid chromatographic method was developed for the analysis of oxolinic acid, flumequine, marbofloxacin and enrofloxacin in honey. These quinolines are unethically used in beekeeping, and a zero-tolerance policy to antibiotic residues in honey has been stated by the European Union. The sample pretreatment was a 1:1 dilution with a 0.05 M SDS at pH 3 solution, filtration and direct injection, thus avoiding extraction steps. The quinolones were eluted without interferences using mobile phase of 0.05 M SDS/12.5% 1-propanol/0.5% triethylamine at pH 3, running at 1 mL/min under isocratic room through a C18 column. The analytes were detected by fluorescence. The method was successfully validated according to the requirements of the European Union Decision 2002/657/EC in terms of: specificity, linearity (r2 > 0.995), limit of detection and decision limit (0.008–0.070 mg/kg), lower limit of quantification (0.02–0.2 mg/kg), detection capability (0.010–0.10 mg/kg), recovery (82.1–110.0%), precision (<9.4%), matrix effects, robustness (<10.4%), and stability. The procedure was applied to several commercial honey supplied by a local supermarket, and the studied antibiotics were not detected. Therefore, the method was rapid, simple, safe, eco friendly, reliable and useful for the routine analysis of honey samples.