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 shu

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

1.
College of Life and Environmental Sciences, Minzu University of China, Beijing 100081, China

Corresponding author: JIN Jun,
Received Date: 6 April 2012
Available Online: 3 June 2012
Fund Project: 本文受到教育部新世纪优秀人才支持计划(No.NCET-10-0106 ) (No.NCET-10-0106 ) 中央民族大学985工程(No.MUC985-9) (No.MUC985-9)中央高校基本科研业务费专项资金中央民族大学自主科研计划项目(No.0910KYQN50)支持 (No.0910KYQN50)

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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沈阳化工大学材料科学与工程学院沈阳 110142