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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
Author(s) -
Jin Micong,
OuYang Xiaokun,
Chen Xiaohong
Publication year - 2006
Publication title -
journal of applied toxicology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.784
H-Index - 87
eISSN - 1099-1263
pISSN - 0260-437X
DOI - 10.1002/jat.1179
Subject(s) - brodifacoum , chromatography , chemistry , electrospray ionization , mass spectrometry , tandem mass spectrometry , selected reaction monitoring , detection limit , high performance liquid chromatography , liquid chromatography–mass spectrometry , triple quadrupole mass spectrometer , rodenticide , organic chemistry
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.