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

An analysis method was developed for the determination of free and bound fractions of polybrominated ethers ( PBDEs) and tetrabromobisphenol A ( TBBPA) in sediment. The free PBDE and TBBPA were extracted with acetone/hexane ( 1∶1) mixed solvent,and the bound fraction was released from the sediment by saponification reaction at 80 ℃. PBDEs and TBBPA were separated via adjusting pH; PBDEs were deter-mined by GC-negative chemical ionization ( NCI) -MS after cleaned up by multilayer silica column,and TBBPA was derivative before pre-separated by acid silica column and finally determined by GC-EI-MS. All of the target compounds were quantitative by internal standard method. The limits of detection of eight low brominated congeners ( BDE28,-47,-66,-100,-99,-154,-153 and -183) ,deca-BDE( BDE209) ,and TBBPA were 0. 6 -12. 5 pg/g,172 pg/g and 4. 2 pg/g,respectively; This method is reliable and stable. The recover-ies of all compounds were ranged from 74% to 106% and the relative standard deviations were below 10%. This method is suitable for the measurement of different forms of PBDEs and TBBPA in sediment under reliable quality assurance and quality control.