Abstract
Bromethalin, a potent neurotoxin, is widely available for use as a rodenticide. As access to other rodenticides is reduced due to regulatory pressure, the use of bromethalin is likely to increase with a concomitant increase in poisonings in nontarget animals. Analytical methods for the detection of bromethalin residues in animals suspected to have been exposed to this rodenticide are needed to support post-mortem diagnosis of toxicosis. This paper describes a novel method for the analysis of desmethylbromethalin (DMB), bromethalin's toxic metabolite, in tissue samples such as liver, brain, and adipose. Samples were extracted with 5% ethanol in ethyl acetate, and an aliquot of the extract was evaporated dry, reconstituted, and analyzed by reverse phase ultrahigh-performance liquid chromatography-mass spectrometry. The mass spectrometer utilized electrospray ionization in negative ion mode with multiple reaction monitoring. This method was qualitatively validated at a level of 1.0 ng/g in liver tissue. The quantitative potential of the method was also evaluated, and a method detection limit of 0.35 ng/g wet weight was determined in fat tissue. DMB was detected in tissue samples from animals suspected to have been poisoned by this compound. To the authors' knowledge, there have been no other methods reported for analysis of DMB in tissue samples using LC-MS/MS.
| Original language | English (US) |
|---|---|
| Pages (from-to) | 5146-5151 |
| Number of pages | 6 |
| Journal | Journal of Agricultural and Food Chemistry |
| Volume | 63 |
| Issue number | 21 |
| DOIs | |
| State | Published - Jun 3 2015 |
Fingerprint
Keywords
- bromethalin
- desmethylbromethalin
- electrospray
- LC-MS/MS
- poisoning
ASJC Scopus subject areas
- Agricultural and Biological Sciences(all)
- Chemistry(all)
Cite this
Method for the detection of desmethylbromethalin in animal tissue samples for the determination of bromethalin exposure. / Filigenzi, Michael S.; Bautista, Adrienne C.; Aston, Linda S.; Poppenga, Robert H.
In: Journal of Agricultural and Food Chemistry, Vol. 63, No. 21, 03.06.2015, p. 5146-5151.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Method for the detection of desmethylbromethalin in animal tissue samples for the determination of bromethalin exposure
AU - Filigenzi, Michael S.
AU - Bautista, Adrienne C.
AU - Aston, Linda S.
AU - Poppenga, Robert H
PY - 2015/6/3
Y1 - 2015/6/3
N2 - Bromethalin, a potent neurotoxin, is widely available for use as a rodenticide. As access to other rodenticides is reduced due to regulatory pressure, the use of bromethalin is likely to increase with a concomitant increase in poisonings in nontarget animals. Analytical methods for the detection of bromethalin residues in animals suspected to have been exposed to this rodenticide are needed to support post-mortem diagnosis of toxicosis. This paper describes a novel method for the analysis of desmethylbromethalin (DMB), bromethalin's toxic metabolite, in tissue samples such as liver, brain, and adipose. Samples were extracted with 5% ethanol in ethyl acetate, and an aliquot of the extract was evaporated dry, reconstituted, and analyzed by reverse phase ultrahigh-performance liquid chromatography-mass spectrometry. The mass spectrometer utilized electrospray ionization in negative ion mode with multiple reaction monitoring. This method was qualitatively validated at a level of 1.0 ng/g in liver tissue. The quantitative potential of the method was also evaluated, and a method detection limit of 0.35 ng/g wet weight was determined in fat tissue. DMB was detected in tissue samples from animals suspected to have been poisoned by this compound. To the authors' knowledge, there have been no other methods reported for analysis of DMB in tissue samples using LC-MS/MS.
AB - Bromethalin, a potent neurotoxin, is widely available for use as a rodenticide. As access to other rodenticides is reduced due to regulatory pressure, the use of bromethalin is likely to increase with a concomitant increase in poisonings in nontarget animals. Analytical methods for the detection of bromethalin residues in animals suspected to have been exposed to this rodenticide are needed to support post-mortem diagnosis of toxicosis. This paper describes a novel method for the analysis of desmethylbromethalin (DMB), bromethalin's toxic metabolite, in tissue samples such as liver, brain, and adipose. Samples were extracted with 5% ethanol in ethyl acetate, and an aliquot of the extract was evaporated dry, reconstituted, and analyzed by reverse phase ultrahigh-performance liquid chromatography-mass spectrometry. The mass spectrometer utilized electrospray ionization in negative ion mode with multiple reaction monitoring. This method was qualitatively validated at a level of 1.0 ng/g in liver tissue. The quantitative potential of the method was also evaluated, and a method detection limit of 0.35 ng/g wet weight was determined in fat tissue. DMB was detected in tissue samples from animals suspected to have been poisoned by this compound. To the authors' knowledge, there have been no other methods reported for analysis of DMB in tissue samples using LC-MS/MS.
KW - bromethalin
KW - desmethylbromethalin
KW - electrospray
KW - LC-MS/MS
KW - poisoning
UR - http://www.scopus.com/inward/record.url?scp=84930645894&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=84930645894&partnerID=8YFLogxK
U2 - 10.1021/jf5052706
DO - 10.1021/jf5052706
M3 - Article
C2 - 25688571
AN - SCOPUS:84930645894
VL - 63
SP - 5146
EP - 5151
JO - Journal of Agricultural and Food Chemistry
JF - Journal of Agricultural and Food Chemistry
SN - 0021-8561
IS - 21
ER -