Simultaneous determination of three alternative flame retardants (dechlorane plus, 1,2-bis(2,4,6-tribromophenoxy) ethane, and decabromodiphenyl ethane) in soils by gas chromatography-high resolution mass spectrometry

A gas chromatography-high resolution mass spectrometry (GC-HRMS) method has been developed for the simultaneous determination of three alternative flame retardants, dechlorane plus (DP), 1,2-bis(2,4,6-tribromophenoxy) ethane (BTBPE), and decabromodiphenyl ethane (DBDPE) in soils. The soil samples were extracted by accelerated solvent extraction, followed by purification with concentrated sulfuric acid partitioning combined with acid-base silica gel column separation. The gas chromatography featured with a thermostable capillary column of short length and a thin stationary phase was operated in pulse injection mode. A double-focusing magnetic sector high resolution mass spectrometer with electron impact ionization was used for quantification of the analytes. The method detection limits were 0.27-0.33 pg for DPs, 0.41 pg for BTBPE, and 36 pg for DBDPE. The mean recoveries for DPs, BTBPE, and DBDPE in spiked soils were 88-107%, 78-97%, and 74-113%, respectively, with relative standard deviations ranging from 5.2% to 18%. The recoveries of (13)C-labeled standards for DPs, BTBPE, and DBDPE in soil samples were 45-110%, 67-118%, and 27-82%, respectively. These results met the acceptable range of labeled standards for analysis of polybrominated diphenyl ethers as specified by the USEPA 1614 method.