title: Gas chromatography-mass spectrometric determination of polybrominated diphenyl ethers in complex fatty matrices from aquaculture activities.
abstract: Gas chromatography coupled to mass spectrometry in negative chemical ionization mode (GC-(NCI)MS) has been applied to the quantification and reliable identification of polybrominated diphenyl ethers (PBDEs) in animal and vegetable samples from aquaculture activities. Matrices analyzed included fish fillet, fish feed, fish oil and linseed oil, their fat content ranged from 5% to 100%. Solid-phase extraction (SPE) (using Florisil and silica cartridges) and normal-phase high performance liquid chromatography were tested for an efficient clean-up in order to obtain sample extracts free of interfering compounds. Combining sulphuric acid digestion and SPE with Florisil led to the highest efficiency in the elimination of interferences from the extracts. The sample procedure developed, together with the application of GC-(NCI)MS for measurement, led to the satisfactory determination of PBDEs at microg kg(-1) levels in complex aquaculture matrices with high lipid content. The use of a short and thin film-thickness fused-silica capillary column allowed to determine the problematic BDE 209 with satisfactory results. Three m/z ions were acquired for each analyte, which ensured a reliable identification of compounds detected in samples.
authors.affiliation: Research Institute for Pesticides and Water (IUPA), Avda Sos Baynat, s/n, University Jaume I, 12071 Castellón, Spain.
authors.forename: Jaime
authors.initials: J
authors.lastname: Nácher-Mestre
authors.forename: Roque
authors.initials: R
authors.lastname: Serrano
authors.forename: Félix
authors.initials: F
authors.lastname: Hernández
authors.forename: Laura
authors.initials: L
authors.lastname: Benedito-Palos
authors.forename: Jaume
authors.initials: J
authors.lastname: Pérez-Sánchez
mesh_terms: D000818:Animals; D017756:Aquaculture; D002851:Chromatography, High Pressure Liquid; D005395:Fish Oils / Q000737:chemistry; D005396:Fish Products / Q000032:analysis; D005399:Fishes / Q000378:metabolism; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D055768:Halogenated Diphenyl Ethers / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification; D008043:Linseed Oil / Q000737:chemistry; D052616:Solid Phase Extraction
chemical_list: D005395:Fish Oils; D055768:Halogenated Diphenyl Ethers; D008043:Linseed Oil