Simultaneous determination of ten anticoagulant rodenticides in tissues by column-switching UHPLC-ESI-MS/MS.
This paper describes the development of a method for the simultaneous determination of ten anticoagulant rodenticides (coumafuryl, warfarin, pindone, coumatetralyl, coumachlor, difenacoum, bromadiolone, brodifacoum, chlorophacinone and flocoumafen) in the liver and kidney based on column-switching liquid chromatography coupled with heated electrospray ionization tandem mass spectrometry. The simple sample preparation includes extraction with methanol. A C18 trapping column was used for online solid-phase extraction before analytical separation with the mobile phase comprising a mixture of 0.1% formic acid in water, methanol and acetonitrile. Chromatographic separation was achieved using a Thermo Hypersil ultra high-performance liquid chromatography (UHPLC) C18 column with the mobile phase consisting of 5 mM ammonium formate buffer (pH = 9) and methanol. The column-switching procedure ensured no matrix effects during electrospray ionization (ESI). Extraction recoveries ranged between 91 and 100% for liver and between 89 and 97% for kidney. The method showed good linearity up to 750 ng g(-1). The limit of detection ranged between 0.001 and 0.022 ng g(-1) for liver and between 0.001 and 0.028 ng g(-1) for kidney. The developed method was successfully used in several animal poisoning cases.
Department of Veterinary Public Health and Animal Welfare, Faculty of Veterinary Hygiene and Ecology, University of Veterinary and Pharmaceutical Sciences Brno, 612 42, Brno, Czech Republic. marsalekp@vfu.cz.
Petr
P
Maršálek
Department of Veterinary Public Health and Animal Welfare, Faculty of Veterinary Hygiene and Ecology, University of Veterinary and Pharmaceutical Sciences Brno, 612 42, Brno, Czech Republic.
Helena
H
Modrá
Department of Veterinary Public Health and Animal Welfare, Faculty of Veterinary Hygiene and Ecology, University of Veterinary and Pharmaceutical Sciences Brno, 612 42, Brno, Czech Republic.
Veronika
V
Doubková
Department of Veterinary Public Health and Animal Welfare, Faculty of Veterinary Hygiene and Ecology, University of Veterinary and Pharmaceutical Sciences Brno, 612 42, Brno, Czech Republic.
Vladimír
V
Večerek
D000818:Animals; D000925:Anticoagulants / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004285:Dogs; D007668:Kidney / Q000737:chemistry*; D057230:Limit of Detection; D008099:Liver / Q000737:chemistry*; D012378:Rodenticides / Q000032:analysis*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D034421:Sus scrofa; D053719:Tandem Mass Spectrometry / Q000379:methods
D000925:Anticoagulants; D012378:Rodenticides
Liquid chromatography; Mass spectrometry; Online SPE; Trapping