Method for the analysis of polybrominated diphenylethers in sediments and biota

Three institutes worked together on the development and improvement of methods for the analysis of polybrominated diphenylethers (PBDEs) in sediments and biota. The methods developed consist of a Soxhlet, Ultra Turrax* (biota) or shake-flask extraction (sediment) using hexane (or pentane)/acetone solvent mixtures, clean-up by alumina column chromatography or by gel permeation chromatography, further clean-up by silica gel column chromatography and treatment with sulphuric acid. Several alternatives for extraction and cleanup yielded similar results. The final determination is performed by GC/NCI-MS in the selected ion mode with m/z values of both Br isotopes (79 and 81 occurring in a 1:1 ratio). For decaBDE the fragments m/z 486.7 and 488.7 were also scanned. The coefficients of variation obtained with this method are between 10 and 35% for individual congeners, and comply at least with the international state-of-the-art for this type of analysis. (C) 2001 Elsevier Science B.V. All rights reserved.