A gas chromatography/high-resolution mass spectrometry (GC/HRMS) method for determination of polybrominated diphenyl ethers in fish

A method for the determination of polybrominated diphenyl ethers (PBDEs) in biota for routine analysis is described. The mass spectroscopic (MS) evalu ation of 23 brominated diphenyl ethers, under electron ionization and elect ron capture negative ion conditions using magnetic sector and quadrupole ma ss spectrometers, showed that high-resolution mass spectrometry (HRMS) unde r electron ionization conditions was the most reliable technique, with high selectivity and adequate sensitivity. The instrument detection limit for t his method ranged for individual congeners between 4.8 and 0.1 pg for 3-bro modiphenyl ether (BDE-2) and 2,3',4,4'-tetrabromodiphenyl ether (BDE-66), r espectively, and method detection limit for each homologue group ranged bet ween 5 pg/g for salmon certified reference material (CRM) and 93 pg/g for l ake trout CRM. The effectiveness of this method was evaluated by analyzing the occurrence of PBDEs in commercially available CRMs comprising Lake Ontario lake trout, Pacific herring, and sockeye salmon. The average coefficients of variation for the replicate analyses of PDBEs in several tissue samples were: 25% fo r lake trout, 36% for Pacific herring, and 34% for sockeye salmon. The aver age deviations in the inter-laboratory study were: 14% for lake trout, 15% for Pacific herring, and 37% for sockeye salmon. Results indicated that the described method, based on gas chromatography/high-resolution mass spectro metry, is reliable for determining PBDE concentrations in biological tissue s. (C) 2001 Elsevier Science Ltd. All rights reserved.