Citation: HE Song-Jie, LI Ming-Yuan, JIN Jun, WANG Ying, HE Chang, BU Yun-Jie, TIAN Yang. Determination of New Halogenated Flame Retardants in Human Serum by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2012, 40(10): 1519-1523. doi: 10.3724/SP.J.1096.2012.20364
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A gel permeation chromatography-gas chromatography-negative chemical ionization-mass spectrometry method (GPC-GC-NCI-MS) was developed for the determination of 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 sample. The serum samples were spiked with 13C12BB-153 and 13C10syn-DP as surrogate internal standard before extracting, and the serum lipid was extracted and mostly removed by gel permeation chromatography. Samples were further 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 monitored ions were as follows: 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 lipid. BB-153 and BTBPE were not detected in all serum samples, and the concentrations of syn-DP and anti-DP were 0.7-9.2 ng/g lipid and 0.6-2.0 ng/g lipid, respectively.
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