title: 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 0.05M SDS at pH 3 solution, filtration and direct injection, thus avoiding extraction steps. The quinolones were eluted without interferences using mobile phase of 0.05M SDS/12.5% 1-propanol/0.5% triethylamine at pH 3, running at 1mL/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 (r(2)>0.995), limit of detection and decision limit (0.008-0.070mg/kg), lower limit of quantification (0.02-0.2mg/kg), detection capability (0.010-0.10mg/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.
authors.affiliation: Química Bioanalítica, QFA, ESTCE, Universitat Jaume I, 12071 Castelló, Spain.
authors.forename: K
authors.initials: K
authors.lastname: Tayeb-Cherif
authors.affiliation: Química Bioanalítica, QFA, ESTCE, Universitat Jaume I, 12071 Castelló, Spain. Electronic address: vicentej@uji.es.
authors.forename: J
authors.initials: J
authors.lastname: Peris-Vicente
authors.affiliation: Química Bioanalítica, QFA, ESTCE, Universitat Jaume I, 12071 Castelló, Spain.
authors.forename: S
authors.initials: S
authors.lastname: Carda-Broch
authors.affiliation: Química Bioanalítica, QFA, ESTCE, Universitat Jaume I, 12071 Castelló, Spain.
authors.forename: J
authors.initials: J
authors.lastname: Esteve-Romero
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D000077422:Enrofloxacin; D005062:European Union; D024841:Fluoroquinolones / Q000032:analysis*; D006722:Honey / Q000032:analysis*; D008823:Micelles; D010093:Oxolinic Acid / Q000032:analysis*; D012680:Sensitivity and Specificity
chemical_list: D024841:Fluoroquinolones; D008823:Micelles; D000077422:Enrofloxacin; C080260:marbofloxacin; D010093:Oxolinic Acid; C012976:flumequine
keywords: 1-Propanol (PubChem CID: 1031); Direct injection; Enrofloxacin (PubChem CID: 71188); Flumequine (PubChem CID: 3374); Honey; Hydrochloric acid (PubChem CID: 313); Marbofloxacin (PubChem CID: 60651); Micellar; Oxolinic acid (PubChem CID: 4628); Phosphate salts (PubChem CID: 24203); Quinolone; Sodium dodecyl sulfate (PubChem CID: 3423265); Triethylamine (PubChem CID: 8471); Validation; Water (PubChem CID: 962)