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Concurrent extraction, clean‐up, and analysis of polybrominated diphenyl ethers, hexabromocyclododecane isomers, and tetrabromobisphenol A in human milk and serum
Author(s) -
Shi Zhixiong,
Wang Yifei,
Niu Piye,
Wang Jiandi,
Sun Zhiwei,
Zhang Shuhua,
Wu Yongning
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201300579
Subject(s) - tetrabromobisphenol a , hexabromocyclododecane , chromatography , chemistry , polybrominated diphenyl ethers , extraction (chemistry) , diphenyl ether , solid phase extraction , fractionation , hexane , brominated flame retardant , residue (chemistry) , fire retardant , organic chemistry , pollutant
A method has been developed and validated for the concurrent extraction, clean‐up, and analysis of polybrominated diphenyl ethers ( PBDE s), α‐, β‐, and γ‐hexabromocyclododecane ( HBCD ), and tetrabromobisphenol A (TBBPA) in human milk and serum. Milk and serum samples were extracted using accelerated solvent extraction with acetone/hexane 1:1, v/v and liquid–liquid extraction with methyl ‐tert ‐butyl ether/hexane 1:1, v/v, respectively. The removal of co‐extracted biogenic materials was achieved by gel permeation chromatography followed by sulfuric acid treatment. The fractionation of the PBDE s and HBCD / TBBPA was performed using a S upelco LC ‐ S i SPE cartridge. The detection of the PBDE s was then performed by GC – MS and that of the HBCD s and the TBBPA was performed using UPLC – MS/MS . The pretreatment procedure was optimized, and the characteristic ions and fragmentation of the analytes were studied by MS or MS/MS . A recovery test was performed using a matrix spiking test at concentrations of 0.05–10 ng/g. The recoveries ranged from 78.6–108.8% with RSD s equal to or lower than 14.04%. The LOD s were 1.8–60 pg/g. The usefulness of the developed method was tested by the analysis of real human samples, and several brominated flame retardants in different samples were detected and analyzed.