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  • A new and simple method to determine trace levels of sulfonamides in honey by high performance liquid chromatography with fluorescence detection.

A new and simple method to determine trace levels of sulfonamides in honey by high performance liquid chromatography with fluorescence detection.

Journal of chromatography. A (2009-06-10)
José Bernal, María Jesús Nozal, Juan José Jiménez, María Teresa Martín, Esther Sanz
摘要

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).

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Sigma-Aldrich
荧光胺, ≥98% (TLC), powder, used for detection of primary amines