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.
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).
authors.affiliation: Laboratory for Integrative Studies in Amphibian Biology, Department of Integrative Biology, University of California, Berkeley, CA, 94720, USA, martin.hansen@berkeley.edu.
authors.forename: Martin
authors.initials: M
authors.lastname: Hansen
authors.forename: Rikke
authors.initials: R
authors.lastname: Poulsen
authors.forename: Xuan
authors.initials: X
authors.lastname: Luong
authors.forename: David L
authors.initials: DL
authors.lastname: Sedlak
authors.forename: Tyrone
authors.initials: T
authors.lastname: Hayes
mesh_terms: D000818:Animals; D001681:Biological Assay / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods; D004781:Environmental Exposure / Q000032:analysis*; D004784:Environmental Monitoring / Q000379:methods; D008099:Liver / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods*; D052616:Solid Phase Extraction / Q000379:methods*; D014230:Triazoles / Q000032:analysis* / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry; D014982:Xenopus laevis / Q000378:metabolism*
chemical_list: D014230:Triazoles; D014874:Water Pollutants, Chemical; C087114:tebuconazole