Development of a cleanup method for polybrominated diphenyl ether (PBDE) in fish by freezing-lipid filtration

A new cleanup method for the determination of brominated flame retardants with an emphasis on polybrominated diphenyl ethers (PBDEs) has been developed for fish tissue sample. This method effectively reduces the sample pretreatment time, labor and required less solvent quantities relative to conventional methods. Freezing-lipid filtration procedure removes approximately 90 % of the lipids in the extract without any significant loss of the PBDEs. A multilayered silica gel column was used for further cleanup of the extracts after freezing-lipid filtration. Multilayered silica gel column chromatography eliminated most of the co-extracted interferences, such as residual lipids and fatty acids. The extracts were analyzed after cleanup by high-resolution gas chromatography/high-resolution mass spectrometry using the isotope dilution method. Tissue samples with 1. 6-8. 0 and 8. 0-40 ppb of PBDE were analyzed using both the sulfuric acid treatment and freezing-lipid filtration cleanup methods in order to evaluate the method performance. Sulfuric acid treatment did not detect 2,4-DiBDE, whereas freezing-lipid filtration detected 2,4-DiBDE but at 50 % recovery. To compare the method, WMF-01 was analyzed via both the sulfuric acid treatment and freezing-lipid filtration cleanup.