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United States Department of Agriculture

Agricultural Research Service

Title: Multiresidue Analysis of Seven Anticoagulant Rodenticides by high-performance liquid chromatography/electrospray/mass spectrometry

Authors
item Marek, Le Etta - MN DEPT OF AGRICULTURE
item Koskinen, William

Submitted to: Journal of Agricultural and Food Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: November 29, 2006
Publication Date: January 4, 2007
Citation: Marek, L.J., Koskinen, W.C. 2007. Multiresidue analysis of seven anticoagulant rodenticides by high-performance liquid chromatography/electrospray/mass spectrometry. Journal of Agricultural and Food Chemistry. 55:571-576.

Interpretive Summary: Mice and rat populations are commonly controlled by two classes of rodenticide anticoagulants, coumarins and indandiones. However, potential poisoning of nontarget animals also often occurs when the anticoagulant rodenticides are misused or are transported from site of intended use. The objective of this study was to develop a multiresidue method for the simultaneous determination of the most commonly used coumarin and indandione anticoagulent rodenticides (i.e. coumafuryl, warfarin, pindone, diphacinone, chlorophacinone, bromadiolone, and brodifacoum) in the matrices most commonly associated with the accidental misuse of the these chemicals, such as in water or animal feed stocks or baits. The developed method must be rapid, have minimal cleanup, and provide the simultaneous detection and confirmation of the seven anticoagulant rodenticides. Using modern analytical instrumentation (liquid chromatograph coupled to a mass spectrometer (LC/ESI/MS/MS)), we developed a method whereby the seven anticoagulant coumarin and indandione rodenticides could be easily separated, confirmed, and quantified. The developed method is relatively rapid. The total time for extraction and sample preparation was < 90 min. The developed method provides the simultaneous quantification and confirmation of the seven anticoagulant rodenticides at trace levels that may be found in variety of types of samples. This method will be beneficial to agencies and laboratories responsible for the identification of sources in suspected poisoning cases involving anticoagulant pesticides in these matrices. In cases such as these, diagnostic laboratories will have the needed rapid, multiresidue method, which provides positive confirmation for both classes of anticoagulant rodenticides that we have developed.

Technical Abstract: Mice and rat populations are commonly controlled by two classes of rodenticide anticoagulants, coumarins and indandiones. However, poisoning of nontarget animals also often occurs. For cases such as these, a rapid, multi-residue method, which provides positive confirmation for both classes of anticoagulant rodenticides is needed by diagnostic laboratories. A method was developed for the determination of seven anticoagulant rodenticides, coumafuryl, pindone, warfarin, diphacinone, chlorophacinone, bromadiolone, and brodifacoum by high performance liquid chromatography/electrospray/mass spectrometry (LC/ESI/MS/MS). Detection was by MS/MS with electrospray ionization in negative mode. Confirmation was by retention time, m/z of molecular ion and two parent- daughter transitions. Recoveries from selected matrices ranged from 61-117%. Detection limits were as low as 1.5-4.5 ng/g. The developed method was rapid and provided the simultaneous quantification and confirmation of the seven anticoagulant rodenticides.

Last Modified: 8/21/2014
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