Analysis of Free and Bound Residues of Polybrominated Diphenyl Ethers and Tetrabromobisphenol A in Sediment

An analysis method was developed for determining free and bound fractions of polybrominated ethers (PBDEs) and tetrabromobisphenol A (TBBPA) in sediments. The free PBDE and TBBPA were extracted with acetone/hexane (1:1, V/V) mixed solvent, and the bound fraction was released from the sediment by saponification at 80 °C. The PBDEs and TBBPA were separated by adjusting pH; PBDEs were determined by GC-NCI-MS after being cleaned up by multilayer silica gel column, and TBBPA was derived before preseparated by acid silica gel column and finally determined by GC-EI-MS. All the target compounds were quantitative by internal standard method. The limits of detection of eight lower brominated congeners (BDE 28, 47, 66, 100, 99, 154, 153, 183), deca-BDE (BDE 209), and TBBPA were 0.6–12.5 pg g−1, 172 and 4.2 pg g−1, respectively. This method is stable and reliable. The recoveries of all compounds were ranged from 74% to 106%, and the relative standard deviations were below 10%. This method appeared to be suitable for the measurement of different forms of PBDEs and TBBPA in sediment under reliable quality assurance and quality control.