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Citation: LI Jian, WANG Yi-Fei, ZHOU Xian-Qing, SHI Zhi-Xiong. Determination of 18 Brominated Flame Retardants in Dairy Product by Gel Permeation Chromatography-Solid Phase Extraction Coupled to Gas Chromatography-Mass Spectrometry and High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(11): 1742-1747. doi: 10.11895/j.issn.0253-3820.160244 shu

Determination of 18 Brominated Flame Retardants in Dairy Product by Gel Permeation Chromatography-Solid Phase Extraction Coupled to Gas Chromatography-Mass Spectrometry and High Performance Liquid Chromatography-Tandem Mass Spectrometry

LI Jian ^1,2, ,
WANG Yi-Fei ^1,2 ,
ZHOU Xian-Qing ^1,2 ,
SHI Zhi-Xiong ^1,2

1.
School of Public Health, Capital Medical University, Beijing 100069, China;
2.
Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing 100069, China

Received Date: 30 March 2016
Revised Date: 23 June 2016

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 21477083)

A novel method was developed for the simultaneous determination of 6 novel brominated flame retardants (NBFRs), 8 polybrominated diphenyl ethers (PBDEs), tetrabromobisphenolA (TBBPA) and α, β, γ-hexabromocyclododecane (α, β, γ-HBCD) in dairy product. Dairy product samples were extracted using soxhlet extraction with acetone/hexane (1:1, V/V). The removal of co-extracted materials was achieved by gel permeation chromatography followed by acidified silica treatment. The fractionation of the PBDEs/NBFRs and HBCD/TBBPA was performed using a Supelco LC-Si SPE cartridge. The detection of the PBDEs and NBFRs was then performed by GC-NCI/MS, and that of the HBCDs and the TBBPA was performed using HPLC-MS/MS. A recovery test was performed using a matrix spiking test and for most of the analytes the recoveries ranged from 80.1% to 114.7% with RSDs equal to or lower than 14.9%. The LODs were 0.2-119.2 pg/g. This methodology was validated to be accurate and sensitive for the simultaneous pretreatment and analysis of brominated flame retardants in dairy product.
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