Rapid and Effective Clean-up Method for PBDE Analysis in Biological and Sediment Samples using a Sulfoxide Cartridge Column

Abstract

An analytical method for the determination of polybrominated diphenyl ethers (PBDEs) in sediment and fish samples has been developed by using a sulfoxide cartridge column as an effective clean-up procedure. After saponification of samples, PBDEs were extracted with hexane. Then the extract was treated with sulfuric acid and frorisil column chromatography. The eluate from the florisil column was loaded on a sulfoxide cartridge column, and then PBDEs were eluted with 20 mL of 10 % acetone/hexane. The measurement of PBDEs was carried out by HRGC-HRMS. By cleaning with a sulfoxide cartridge column, the number of peaks on SIM chromatograms that cause the drop of lock mass signal during GC-MS measurement and interfere with the quantification of PBDEs was dramatically reduced. The developed method was applied to the analysis of certificated reference materials of fish tissue and soil. The results obtained were within the range of certificated values except for 2,2′,3,4,4′,5′,6-heptabromodiphenyl ether (#183).