Determination of the rodenticide difenacoum in biological materials by high-pressure liquid chromatography with confirmation of identity by mass spectrometry

Superwarfarins

“…Early HPLC methods focused on an individual chemical. For example, methods to detect chlorophacinone in formulations (Grant and Pike, 1979;Vigh et al, 1981), brodifacoum in serum (Murphy and Gerken, 1989), brodifacoum (Koubek et al, 1979;Keiboom and Rammel, 1981;Hoogenboom and Rammell, 1983;Ray et al, 1989), bromadiolone (Hunter, 1983;Subbiah et al, 2005), chlorophacionone (Hunter, 1985), difethiolone (Goldade et al, 1998), and difenacoum (Mundy and Machin, 1977) in tissue have been reported.…”

The emerging threat of superwarfarins: history, detection, mechanisms, and countermeasures

“…However, owing to their larger mass and lower volatility, superwarfarins such as DiF and BDF are less amenable to analysis using gas chromatography and have been measured instead using thin layer chromatography (TLC) or HPLC . One of the first methods developed used a clean‐up step that incorporated exclusion chromatography using porous glass beads to eliminate macromolecules, followed by HPLC separation and molecular identification by mass spectrometry . Sample preparation for both warfarin and superwarfarins usually uses extraction with organic solvents or, less commonly, solid phase extraction.…”

“…36 One of the first methods developed used a clean-up step that incorporated exclusion chromatography using porous glass beads to eliminate macromolecules, followed by HPLC separation and molecular identification by mass spectrometry. 37 Sample preparation for both warfarin and superwarfarins usually uses extraction with organic solvents or, less commonly, solid phase extraction. Because superwarfarins are more hydrophobic than warfarin and form few polar metabolites, nonpolar organic solvents are particularly useful for their extraction.…”

HPLC Determination of Anticoagulant Rodenticide Residues in Animal Livers

“…A number of HPLC methods have been described for the determination of individual coumarin-based anticoagulants in biological materials including methods for warfarin (Mundy et al 1976, Lee et al 1981, de Vries et al 1993, difenacoum (Mundy et al 1977, Kelly et al 1993) and brodifacoum (Koubek et al 1979, Kieboom et al 1981, Hogenboom et al 1983). Multiresidue methods have also been described: Mundy and Machin (1982) used HPLC to determine four coumarin anticoagulants, but difenacoum, brodifacoum and coumatetralyl were not resolved and had to be identified by further HPLC analysis of the fractions from the column.…”