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

✍ Scribed by Mi-cong Jin; Xiao-kun OuYang; Xiao-hong Chen

• Publisher: John Wiley and Sons
• Year: 2006
• Tongue: English
• Weight: 229 KB
• Volume: 27
• Category: Article
• ISSN: 0260-437X
• DOI: 10.1002/jat.1179

✦ Synopsis

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. Copyright © 2006 John Wiley & Sons, Ltd.