
Gas chromatography-mass spectrometry instrument for the quantification of warfarin metabolites
Source: BAM
Warfarin has been used worldwide since the 1950s both as a prescription drug and as a rodenticide (rat poison). Research has shown that it accumulates in the environment and in the food chain. However, pollutants such as warfarin are also subject to degradation by biotic and abiotic processes and advanced oxidation processes. Therefore, a method for the accurate quantification of warfarin and its metabolites and transformation products in environmental compartments such as water and soil was developed. In addition, a comprehensive investigation of the degradation of warfarin in aqueous solutions by the Fenton reaction using advanced analytical techniques was presented. The Fenton reaction is a reaction of hydrogen peroxide catalysed by iron (II) ions to form reactive hydroxyl radicals, which can be used to simulate degradation processes in the environment. The Fenton’s reaction role in warfarin degradation was investigated, demonstrating that increased hydrogen peroxide concentration accelerates the degradation rate. A gas chromatography-tandem mass spectrometric (GC-MS/MS) method was developed to quantify warfarin and the most typical mono-hydroxylated transformation products. The derivatisation yield of warfarin for in-liner derivatisation with trimethyl-3-trifluoromethyl phenyl ammonium hydroxide (m-TFPTAH) was determined. This method provides an alternative to common LC-MS (liquid chromatography with mass spectrometric detection) techniques for determining warfarin and its mono-hydroxylated metabolites. The method was used successfully to show that the metabolite 4'-O-Me-warfarin is preferentially formed under the given experimental conditions. In addition, a solid-phase-extraction (SPE) step was established to enrich the target analytes. For the first time, GC-EI-(electron impact) induced high-resolution quadrupole time-of-flight mass spectrometric (HR-QToF-MS) data of in-liner derivatised warfarin and selected hydroxylated species is provided as an alternative to common LC-MS/MS approaches.
Developing a GC-EI-MS/MS method for quantifying warfarin and five hydroxylated metabolites generated by the Fenton reaction
Wipert Jannik von Törne, Urszula-Anna Klyk-Seitz & Christian Piechotta
Environmental Science and Pollution Research, Volume 31, Issue 41, 2024