Title: Liquid chromatography tandem mass spectrometry method using solid-phase extraction and bead-beating-assisted matrix solid-phase dispersion to quantify the fungicide tebuconazole in controlled frog exposure study: analysis of water and animal tissue.

Authors: Hansen, Martin; Poulsen, Rikke; Luong, Xuan; Sedlak, David L; Hayes, Tyrone

Published In Anal Bioanal Chem, (2014 Nov)

Abstract: This paper presents the development, optimization, and validation of a LC-MS/MS methodology to determine the concentration of the antifungal drug and fungicide tebuconazole in a controlled exposure study of African clawed frogs (Xenopus laevis). The method is validated on animal tank water and on tissue from exposed and non-exposed adult X. laevis. Using solid-phase extraction (SPE), the analytical method allows for quantification of tebuconazole at concentrations as low as 3.89 pg mL(-1) in 10 mL water samples. Using bead-beating-assisted matrix solid-phase dispersion (MSPD), it was possible to quantify tebuconazole down to 0.63 pg mg(-1) wet weight liver using 150 mg tissue. The deuterated analogue of tebuconazole was used as internal standard, and ensured method accuracy in the range 80.6-99.7% for water and 68.1-109% for tissue samples. The developed method was successfully applied in a 4-week X. laevis repeated-exposure study, revealing high levels of tebuconazole residues in adipose and liver tissue, and with experimental bioconcentration factors up to 18,244 L kg(-1).

PubMed ID: 25277103

MeSH Terms: Animals; Biological Assay/methods; Chromatography, Liquid/methods; Environmental Exposure/analysis*; Environmental Monitoring/methods; Liver/chemistry*; Mass Spectrometry/methods*; Solid Phase Extraction/methods*; Triazoles/analysis*; Triazoles/chemistry; Water Pollutants, Chemical/analysis*; Water Pollutants, Chemical/chemistry; Xenopus laevis/metabolism*