| 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. |
| Authors | Mi-Cong Jin, Xiao-Kun OuYang, Xiao-hong Chen
(Affiliation: Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China. jmcjc at nbip.net)
|
| Journal | Journal of applied toxicology : JAT
(J Appl Toxicol)
2007 Jan-Feb
Vol. 27
Issue 1
Pg. 18-24
ISSN: 0260-437X England |
| PMID | 17177169
(Publication Type: Journal Article, Research Support, Non-U.S. Gov't, Validation Studies)
|
| Copyright | Copyright 2006 John Wiley & Sons, Ltd. |
| Chemical References |
- 4-Hydroxycoumarins
- Anticoagulants
- bromfenacoum
- Warfarin
- flocoumafen
|
| 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)
|
