title: A comprehensive gas chromatography coupled to high resolution mass spectrometry based method for the determination of polybrominated diphenyl ethers and their hydroxylated and methoxylated metabolites in environmental samples.
abstract: We report here an efficient and comprehensive analytical methodology based on gas chromatography with high resolution mass spectrometry (GC-HRMS) to simultaneously determine PBDEs from mono to deca brominated and hydroxy (OH-) and methoxy (MeO-) PBDE metabolites in environmental samples, particularly, sediment, fish tissue and milk. Among a number of extraction and clean-up methods tested, pressurized liquid extraction followed by gel permeation chromatography and florisil clean-up proved to be simple, robust and optimized so that all target analytes (parent compounds and metabolites) were collected in a single fraction. Extracts were analyzed by GC-HRMS to identify PBDEs. Following, the same extracts were derivatized and re-analyzed by GC-HRMS to determine 11 target and 35 non-target OH- and MeO-PBDEs. Monitoring of the M(+) for MeO-PBDEs and the [M-CH(2)CO](+) ions for derivatized OH-PBDEs at 10,000 resolution permitted unequivocal identification of the PBDE metabolites in the environmental matrices examined. The method was validated in terms of accuracy, precision, detection limits and long-term stability. The analytical precision obtained with this method was between 0.3 and 17%, and the limits of quantification were lower than 3.28 pg/g dry weight, 20.5 and 41.4 pg/g lipid weight in sediment, milk and fish, respectively. The method was applied to determine PBDEs and target and non-target metabolites in all three matrices.
authors: Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18-26, 08034 Barcelona, Catalonia, Spain. slbqam@cid.csci.es
authors: S
authors: S
authors: Lacorte
authors: M G
authors: MG
authors: Ikonomou
authors: M
authors: M
authors: Fischer
mesh_terms: D000818:Animals; D004355:Drug Stability; D004785:Environmental Pollutants / Q000032:analysis* / Q000493:pharmacokinetics; D005399:Fishes / Q000378:metabolism*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D019015:Geologic Sediments / Q000737:chemistry*; D055768:Halogenated Diphenyl Ethers / Q000032:analysis*; D006801:Humans; D006900:Hydroxylation; D016014:Linear Models; D008895:Milk, Human / Q000737:chemistry* / Q000378:metabolism; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D004785:Environmental Pollutants; D055768:Halogenated Diphenyl Ethers