4.6 Article

Confirmation of 13 sulfonamides in honey by liquid chromatography-tandem mass spectrometry for monitoring plans: Validation according to European Union Decision 2002/657/EC

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1339, Issue -, Pages 128-136

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2014.03.003

Keywords

Sulfonamides; Antibiotics; Residues; Honey; Analysis; Liquid chromatography/mass spectrometry; (LC-MS/MS)

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A rapid and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous confirmation of 13 sulfonamides in honey was developed and fully validated in accordance with the European Commission Decision No 2002/657/EC. The validation scheme was built in accordance with the target level of 50 mu g kg(-1) for all analytes. The sulfonamides investigated were as follows: sulfaguanidine (SGN), sulfanilamide (SNL), sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethizole (SMZ), sulfadimerazine (SDM), sulfamonomethoxine (SMNM), sulfamethoxypiridazine (SMP), sulfadoxine (SDX), sulfamethoxazole (SMX), sulfaquinoxaline (SQX) and sulfadimethoxine (SOT). Several extraction procedures were investigated during the development phase. Finally, the best results were obtained with a procedure using acidic hydrolysis and cation exchange purification. Chromatographic separation was achieved on a C18 analytical column. Matrix effects were also investigated. Data acquisition implemented for the confirmatory purpose was performed by monitoring 2 MRM transitions per analyte under the positive electrospray mode. Mean relative recoveries ranged from 85.8% to 110.2% and relative standard deviations lying between 2.6% and 19.8% in intra-laboratory reproducibility conditions. The decision limits (CC alpha) ranged from 1.8 to 15.5 mu g kg(-1). High resolution mass spectrometry was used to investigate the possible formation of sulfonamide metabolites in honey. The validation results proved that the method is suitable for the screening and confirmatory steps as implemented for the French monitoring residue plan for sulfonamides residue control in honeybees. (C) 2014 Elsevier B.V. All rights reserved.

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