title: Sample preparation method for the speciation of polybrominated diphenyl ethers and their methoxylated and hydroxylated analogues in diverse environmental matrices.
abstract: A reliable analytical method was developed here for the simultaneous separation, identification and quantification of ten polybrominated diphenyl ethers (PBDEs), nine methoxylated PBDEs (MeO-PBDEs) and ten hydroxylated PBDEs (OH-PBDEs) in various environmental matrices, including water, soil, sediment, plant, mollusk and fish. PBDEs and MeO-PBDEs were measured by gas chromatography coupled with mass spectrometry (GC/MS) and liquid chromatography coupled with electrospray ionization (negative)-tandem quadrupole mass spectrometry (LC/ESI(-)-MS/MS) for the separation and determination of OH-PBDEs without prior derivatization. After preliminary sample cleaning using acid silica gel, water-impregnated silica column separation of PBDEs, MeO-PBDEs and OH-PBDEs was proved to be rapid, simple, and efficient. For phenolic analytes, the method detection limits (MDLs) were 3.2-11.6pg/L in water sample and 2.8-18.4pg/g dry weight in solid samples. For neutral compounds, MDLs were 48.8-150.3pg/L in water sample and 46.5-170.8pg/g dry weight in solid samples. The method was validated using six kinds of environmental samples spiked with all analytes at three concentration levels (0.3ng, 2ng and 5ng, respectively) for recovery (71-113%) and repeatability determination (4-12%RSD).
authors.affiliation: State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085, China.
authors.forename: Jianteng
authors.initials: J
authors.lastname: Sun
authors.forename: Jiyan
authors.initials: J
authors.lastname: Liu
authors.forename: Qian
authors.initials: Q
authors.lastname: Liu
authors.forename: Guangbo
authors.initials: G
authors.lastname: Qu
authors.forename: Ting
authors.initials: T
authors.lastname: Ruan
authors.forename: Guibin
authors.initials: G
authors.lastname: Jiang
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid; D004785:Environmental Pollutants / Q000032:analysis; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry; D019015:Geologic Sediments / Q000737:chemistry*; D055768:Halogenated Diphenyl Ethers / Q000032:analysis*; D006900:Hydroxylation; D057230:Limit of Detection; D008974:Mollusca / Q000737:chemistry*; D015203:Reproducibility of Results; D058428:Silica Gel; D012987:Soil / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry; D014867:Water / Q000737:chemistry*
chemical_list: D004785:Environmental Pollutants; D055768:Halogenated Diphenyl Ethers; D012987:Soil; D014867:Water; D058428:Silica Gel