Development of analytical procedures for the simultaneous determination of tri- to heptabrominated diphenyl ethers and hexabrominated biphenyl (BB 153) in sediment samples

Abstract

A simple analytical procedure was developed for simultaneous determination of trace levels of tri- to hepta-BDEs as well as 2,2′,4,4′,5,5′-hexabromobiphenyl (BB 153). The mechanical shaking extraction technique for the isolation of target analytes was optimised. Different extraction solvent combinations were tested under different extraction time periods of 3, 6, 12 and 16 h. The n-hexane:acetone (2:1, v/v) combination gave the best recovery at the optimum extraction of 12 h. Target analytes were quantified using a high capillary gas chromatograph (GC) equipped with an electron capture detector. Under the optimum GC conditions, the resolution of the co-eluting BDE 154 and BB 153 was achieved. The overall recoveries of target analytes in the matrix spike experiment conducted ranged between 84.4 and 110% for BDE 183 and BDE 28, respectively. The method was applied to 19 field sediment samples collected from a control site and from 3 sampling locations (upstream, point of discharge and downstream) of the Black River, which receives effluent from a wastewater treatment plant (WWTP). The sum of the mean concentrations of all of the 7 PBDE congeners was 4.63, 0.35, 'not detectable' and 4.43 ng/g, for the control site, upstream, point of discharge and downstream samples, respectively. The concentrations of BB 153 were generally low in these samples and ranged between ND and 0.89 ng/g. The developed method allows for the simultaneous determination of PBDE congeners and BB 153. It is efficient, moderately rapid and cost-effective.