Analysis of sulfonamide residues in real honey samples using liquid chromatography with fluorescence and tandem mass spectrometry detection

Ádám Tölgyesi, Róbert Berky, Katalin Békési, Szabolcs Fekete, Jenõ Fekete, Virender K. Sharma

Research output: Contribution to journalArticle

15 Citations (Scopus)

Abstract

This paper presents new reversed phase liquid chromatographic methods (HPLC-FLD and LC-MS/MS) for the quantification of sulfonamides in spiked and incurred honey samples. The sample preparation was optimized using Oasis HLB (hydrophilic-lipophilic balance) solid-phase extraction (SPE) cartridge. Elutions of sulfonamides were carried out under acidic, neutral, and basic conditions using methanol. Recoveries under acid condition were in the range from 66.8-90%, which were approximately 10% higher than those obtained under other conditions. The sample clean-up was also tested using Strata-XL cartridges. The HPLC-FLD separation was performed using a Varian C18 column and a ternary (methanol-acetonitrile-phosphate buffer, pH 5) mobile phase resulting good selectivity for the determination. The robustness of the ternary gradient method was evaluated by computer simulation (DryLab). LC-MS/MS separation was carried out on a Kinetex XB core-shell type HPLC column that enabled a low limit of detection (0.01-0.5 μg/kg) and faster separation (6 min). The developed methods were validated in accordance with the European Union Commission Decision 2002/657/EC and were applied successfully for more than four hundred honey samples (under a national monitoring program). The concentrations of sulfadimethoxine, sulfachloropyridazine, and trimethoprim residues in samples were found in a concentration range from 0.03 up to 686 μg/kg.

Original languageEnglish
Pages (from-to)1105-1125
Number of pages21
JournalJournal of Liquid Chromatography and Related Technologies
Volume36
Issue number8
DOIs
Publication statusPublished - Mar 1 2013

Keywords

  • DryLab software
  • High performance liquid chromatography
  • Honey
  • Kinetex XB HPLC column
  • Optimization
  • Sulfonamides

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Pharmaceutical Science
  • Clinical Biochemistry

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