Sample preparation method for the speciation of polybrominated diphenyl ethers and their methoxylated and hydroxylated analogues in diverse environmental matrices

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 3.2–11.6 pg/L in water sample and 2.8–18.4 pg/g dry weight in solid samples. For neutral compounds, MDLs were 48.8–150.3 pg/L in water sample and 46.5–170.8 pg/g dry weight in solid samples. The method was validated using six kinds of environmental samples spiked with all analytes at three concentration levels (0.3 ng, 2 ng and 5 ng, respectively) for recovery (71–113%) and repeatability determination (4–12%RSD).