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

Anal Chim Acta. 2008 Apr 14;613(1):98-107. doi: 10.1016/j.aca.2008.02.045. Epub 2008 Feb 29.

Abstract

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 (CCalpha), detection capability (CCbeta), 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.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Chromatography, Liquid / methods*
  • Chromatography, Liquid / standards
  • Enrofloxacin
  • European Union
  • Fluorescence
  • Fluoroquinolones / chemistry
  • Linear Models
  • Milk / chemistry*
  • Quinolones / analysis*
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Solid Phase Extraction
  • Tandem Mass Spectrometry / methods*
  • Tandem Mass Spectrometry / standards
  • Ultraviolet Rays

Substances

  • Fluoroquinolones
  • Quinolones
  • Enrofloxacin