title: Gas chromatography-ion trap tandem mass spectrometry method for the analysis of methoxylated polybrominated diphenyl ethers in fish.
abstract: Gas chromatography coupled to ion trap tandem mass spectrometry (GC-ITMS-MS) is proposed for the analysis of methoxylated polybrominated diphenyl ethers (MeO-PBDEs) in fish and shellfish. MS-MS operating parameters related to the isolation and fragmentation of the precursor ions were optimized to achieve maximum sensitivity and selectivity. This new method allows the determination of both MeO-PBDEs and PBDEs in a single run. Low limits of detection (0.4-2.5 pg injected) and high precision (RSD<13%) were achieved. A sample treatment based on a selective pressurized liquid extraction (PLE) using Florisil as fat retainer was applied for the analysis of these compounds in fish samples. Method limits of quantification ranged from 0.11 to 0.95 ng g(-1) lipid weight for MeO-PBDEs and between 0.18 and 0.50 ng g(-1) lipid weight for PBDEs. In addition, good repeatability of the whole method was achieved (RSD<15%). The suitability of the method was evaluated by analyzing a certified reference material (SRM 1945, whale blubber) with satisfactory results. The developed method was applied to the simultaneous analysis of MeO-PBDEs and PBDEs in fish and shellfish samples from the Mediterranean Sea.
authors.affiliation: Department of Analytical Chemistry, University of Barcelona. Avda. Diagonal 647, E-08028 Barcelona, Spain.
authors.forename: S
authors.initials: S
authors.lastname: Losada
authors.forename: F J
authors.initials: FJ
authors.lastname: Santos
authors.forename: A
authors.initials: A
authors.lastname: Covaci
authors.forename: M T
authors.initials: MT
authors.lastname: Galceran
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry*; D005591:Chemical Fractionation; D004785:Environmental Pollutants / Q000032:analysis / Q000737:chemistry; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D055768:Halogenated Diphenyl Ethers / Q000032:analysis* / Q000737:chemistry; D008055:Lipids / Q000737:chemistry; D009132:Muscles / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry
chemical_list: D004785:Environmental Pollutants; D055768:Halogenated Diphenyl Ethers; D008055:Lipids