Simultaneous determination of ten anticoagulant rodenticides in tissues by column-switching UHPLC-ESI-MS/MS

Anal Bioanal Chem. 2015 Oct;407(25):7849-54. doi: 10.1007/s00216-015-8954-1. Epub 2015 Aug 18.

Abstract

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.

Keywords: Liquid chromatography; Mass spectrometry; Online SPE; Trapping.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Animals
  • Anticoagulants / analysis*
  • Chromatography, High Pressure Liquid / methods*
  • Dogs
  • Kidney / chemistry*
  • Limit of Detection
  • Liver / chemistry*
  • Rodenticides / analysis*
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Sus scrofa
  • Tandem Mass Spectrometry / methods

Substances

  • Anticoagulants
  • Rodenticides