title: A new and simple method to determine trace levels of sulfonamides in honey by high performance liquid chromatography with fluorescence detection.
abstract: A novel method for the simultaneous analysis at trace level of sulfonamides (sulfaguanidine, sulfanilamide, sulfacetamide, sulfathiazole, sulfapyridine, sulfachloropyridazine, sulfamerazine, sulfameter, sulfamethazine, sulfadoxine, sulfadiazine, sulfamonomethoxine, sulfadimethoxine) in honey is described. Methanol has been used in the sample treatment step to avoid the emulsion formation and to break the N-glycosidic bond between sugars and sulfonamides. The determination is carried out by liquid chromatography in gradient elution mode, with fluorescence detection after the on-line pre-column derivatization with fluorescamine. The influence of parameters such as the mobile phase composition, column temperature, pH or injection volume, on the separation has been taken into account and the derivatization step has also been optimized. Recoveries of the compounds on spiked honey samples ranged from 56% for sulfadoxine to 96% for sulfacetamide, with relative standard deviations below 10%. The quantitation limits are between 4 and 15 ng g(-1).
authors.affiliation: Institute of Industrial Fermentations (CSIC), Juan de la Cierva 3, 28006 Madrid, Spain. jbernal@ifi.csic.es
authors.forename: José
authors.initials: J
authors.lastname: Bernal
authors.forename: María Jesús
authors.initials: MJ
authors.lastname: Nozal
authors.forename: Juan José
authors.initials: JJ
authors.lastname: Jiménez
authors.forename: María Teresa
authors.initials: MT
authors.lastname: Martín
authors.forename: Esther
authors.initials: E
authors.lastname: Sanz
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005450:Fluorescamine / Q000737:chemistry; D005453:Fluorescence; D006722:Honey / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D000432:Methanol / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013449:Sulfonamides / Q000032:analysis*; D013696:Temperature
chemical_list: D013449:Sulfonamides; D005450:Fluorescamine; D000432:Methanol