Environmental analytical methods

Simultaneous determination of brominated phenols in soils

Wei Han , Sen Wang , Honglin Huang , Lei Luo , Shuzhen Zhang


Received January 23, 2013,Revised April 15, 2013, Accepted , Available online November 01, 2013

Volume ,2013,Pages 2306-2312

Brominated phenols (BPs), a widely used group of emerging flame retardants, are important environmental contaminants and exhibit endocrine disrupting potential. Method for simultaneous determination of tetrabromobisphenol A (TBBPA), tribromophenol (TBP), dibromophenols (DBPs) and monobromophenols (MBPs) in soils using gas chromatography-mass spectrometry analysis (GC/MS) was successfully developed. Cleanup methods for soil extracts including several solid-phase extraction cartridges and different elution solvents were compared and optimized. Florisil cartridge with dichloromethane as the elution reagent was selected for sample cleanup owing to its high and reproducible recoveries of the target analytes in soils. Derivatization conditions were tested and the optimal conditions were obtained with 20 μL silylation reagent at room temperature. The chromatographic separation was optimized with different columns and DB-XLB column was selected for its excellent separation of the analytes. The limits of detection for the target compounds were from 0.04 to 0.19 ng/g. Mean recoveries of the compounds from spiked soils exceeded 84% with a good reproducibility, excepting that the recovery of 2-bromophenol was relatively poor (lower than 55%) due to its instability. The developed method was applied to the determination of the BPs in the soils collected from e-waste sites. The contents of BPs in the soils were at ng/g levels with TBBPA and TBP the most frequently detected. To our knowledge, this is the first report for the simultaneous determination of TBBPA, TBP, DBPs and MBPs in soils.

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