Improved determination of quinolones in milk at their MRL levels using LC-UV, LC-FD, LC-MS and LC-MS/MS and validation in line with regulation 2002/657/EC

Heymo M. P., NEMUTLU E., Kir S., Barron D., Barbosa J.

ANALYTICA CHIMICA ACTA, vol.613, no.1, pp.98-107, 2008 (SCI-Expanded) identifier identifier identifier

  • Publication Type: Article / Article
  • Volume: 613 Issue: 1
  • Publication Date: 2008
  • Doi Number: 10.1016/j.aca.2008.02.045
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Page Numbers: pp.98-107
  • Keywords: milk, quinolones, EU criteria, liquid chromatography-ultraviolet detection, liquid chromatography-fluorescence detection, liquid chromatography-mass spectrometry, liquid chromatography-tandem mass spectrometry, TANDEM MASS-SPECTROMETRY, PERFORMANCE LIQUID-CHROMATOGRAPHY, SOLID-PHASE EXTRACTION, FLUORESCENCE DETECTION, MULTIRESIDUE DETERMINATION, BOVINE-MILK, CAPILLARY-ELECTROPHORESIS, METABOLITE CIPROFLOXACIN, ANTIBACTERIAL AGENTS, ANIMAL-TISSUES
  • Hacettepe University Affiliated: Yes


This paper reports the multi-residue determination of quinolones included in the European Union regulations (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin and flumequine) in bovine milk, using liquid chromatography with ultraviolet (LC-UV), fluorescence (LC-FD), mass spectrometry (LC-MS) and tandem mass spectrometry detection (LC-MS/MS). The methods were validated, in line with EU requirements (Commission Decision 2002/657/EC). Linearity, decision limit (CC alpha), detection capability (CC beta), detection limit (LOD), quantification limits (LOQ), recoveries, precision, selectivity and stability were determined and adequate results were obtained. Recoveries higher than 80% were obtained for all quinolones. The methods developed were used to quantify enrofloxacin and its main metabolite, ciprofloxacin, in milk from animals treated with enrofloxacin. (C) 2008 Elsevier B.V. All rights reserved.