Determination and confirmation of chloramphenicol in honey, fish and prawns by liquid chromatography-tandem mass spectrometry with minimum sample preparation: validation according to 2002/657/EC Directive

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(4):550-8. doi: 10.1080/19440049.2011.641160. Epub 2012 Jan 12.

Abstract

A reliable, simple and sensitive liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) confirmation method has been developed for chloramphenicol (CAP) determination in honey, fish and prawns. For honey, samples were extracted with ethyl acetate, an aliquot was evaporated to dryness and re-dissolved in mobile phase. For fish and prawns, tissues were extracted with acetonitrile and chloroform. The organic layer was evaporated to dryness and the residue was re-constituted with water: acetonitrile (90:10). LC separation was achieved on a C18 column with gradient elution using a mobile phase of acetonitrile and water. Analysis was carried out on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring (MRM) mode via electrospray interface operated in negative ionisation mode, with deuterated chloramphenicol-d(5) (d(5)-CAP) as internal standard. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Four identification points were obtained for CAP with one precursor ion and two product ions. The limit of detection (LOD) was 0.02 µg kg(-1). Linear calibration curves were obtained over concentration ranges of 0.1-1.0 µg kg(-1) in tissues. Mean recoveries ranged from 85.5% to 115.6%, with the corresponding intra- and inter-day variation ranging from 1.0% to 22.5%, depending on matrix type and level of concentration. The decision limit (CCα) and detection capability (CCβ) of the method were obtained for all matrices: 0.04 and 0.06 µg kg(-1), respectively, for prawns and fish and 0.05 and 0.09 µg kg(-1) for honey.

Publication types

  • Validation Study

MeSH terms

  • Animals
  • Chloramphenicol / analysis*
  • Chromatography, Liquid / methods*
  • Drug Residues / analysis*
  • European Union
  • Fishes
  • Food Contamination / analysis*
  • Food Contamination / legislation & jurisprudence
  • Food Contamination / statistics & numerical data
  • Honey / analysis
  • Limit of Detection
  • Seafood / analysis
  • Shellfish / analysis
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Tandem Mass Spectrometry / methods*
  • Veterinary Drugs / analysis

Substances

  • Veterinary Drugs
  • Chloramphenicol