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High-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry for the determination of flocoumafen and brodifacoum in whole blood.

Abstract
A high-performance liquid chromatographic-tandem mass spectrometric (HPLC-MS-MS) assay was developed and validated to determine quantitatively flocoumafen and brodifacoum in whole blood using warfarin as an internal standard (IS). Liquid-liquid extraction, using ethyl acetate, was used to isolate flocoumafen, brodifacoum and the IS from the biological matrix. Detection was performed on a mass spectrometer by negative electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The calibration curves were linear (r(2) > 0.998) in the concentration range of 0.1-100.0 ng ml(-1) with a lower limit of quantification of 0.05 ng ml(-1) for flocoumafen, and 0.1 ng ml(-1) for brodifacoum in whole blood. Intra-day and inter-day relative standard deviations (RSDs) were less than 8.0% and 10.8%, respectively. Recoveries of flocoumafen and brodifacoum ranged from 78.0% to 83.7%. This assay can be used to determine trace flocoumafen and brodifacoum in whole blood to investigate suspected poisoning of human and animals.
AuthorsMi-Cong Jin, Xiao-Kun OuYang, Xiao-hong Chen
JournalJournal of applied toxicology : JAT (J Appl Toxicol) 2007 Jan-Feb Vol. 27 Issue 1 Pg. 18-24 ISSN: 0260-437X [Print] England
PMID17177169 (Publication Type: Journal Article, Research Support, Non-U.S. Gov't, Validation Study)
CopyrightCopyright 2006 John Wiley & Sons, Ltd.
Chemical References
  • 4-Hydroxycoumarins
  • Anticoagulants
  • flocoumafen
  • Warfarin
  • bromfenacoum
Topics
  • 4-Hydroxycoumarins (blood, chemistry)
  • Anticoagulants (blood, chemistry)
  • Chromatography, High Pressure Liquid (methods, standards)
  • Drug Monitoring (methods)
  • Drug Stability
  • Forensic Toxicology (methods)
  • Humans
  • Reference Standards
  • Reproducibility of Results
  • Spectrometry, Mass, Electrospray Ionization (methods, standards)
  • Tandem Mass Spectrometry (methods, standards)
  • Warfarin (blood)

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