Determination of New Halogenated Flame Retardants in Human Serum by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry

A Gel permeation chromatography-Gas chromatography-negative chemical ionization-mass spectrometry method (GPC-GC-NCI-MS) was developed to measure 2,2′,4,4′,5,5′-hexabromobiphenyl (BB-153), 1,2-bis(2,4,6-tribromophenoxy) ethane (BTBPE) and dechlorane plus (DP) in human serum samples. The serum samples were spiked with 13C12BB-153 and 13C10syn-DP as surrogate internal standard before extracting, and the serum lipid was extracted and removed by gel permeation chromatography. Then the samples were cleaned up with a silica/sulfuric acid column. Identification and quantification of BB-153, BTBPE, syn-DP and anti-DP were performed by Gas chromatography-negative chemical ionization-mass spectrometry. The following ions were monitored: m/z 627.5 and 629.5 for BB-153; m/z 79 and 81 for BTBPE; m/z 652 and 654 for DP. The recoveries of 13C12BB-153 and 13C10syn-DP in serum samples were 91.5% ± 8.9% and 92.3% ± 8.1%, respectively. The limits of detection were from 0.6 to 1.2 ng g−1 lipid. BB-153 and BTBPE were not detected in all the serum samples, and the concentrations of syn-DP and anti-DP were 0.7–9.2 ng g−1 lipid and 0.6–2.0 ng g−1 lipid, respectively.