Concurrent extraction, clean-up, and analysis of polybrominated diphenyl ethers, hexabromocyclododecane isomers, and tetrabromobisphenol A in human milk and serum.
A method has been developed and validated for the concurrent extraction, clean-up, and analysis of polybrominated diphenyl ethers (PBDEs), 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 PBDEs and HBCD/TBBPA was performed using a Supelco LC-Si SPE cartridge. The detection of the PBDEs was then performed by GC-MS and that of the HBCDs 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 RSDs equal to or lower than 14.04%. The LODs 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.
School of Public Health, Capital Medical University, Beijing, China; Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
Zhixiong
Z
Shi
Yifei
Y
Wang
Piye
P
Niu
Jiandi
J
Wang
Zhiwei
Z
Sun
Shuhua
S
Zhang
Yongning
Y
Wu
D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D055768:Halogenated Diphenyl Ethers / Q000097:blood / Q000737:chemistry* / Q000302:isolation & purification; D006801:Humans; D006842:Hydrocarbons, Brominated / Q000097:blood / Q000737:chemistry* / Q000302:isolation & purification; D007536:Isomerism; D008895:Milk, Human / Q000737:chemistry*; D011075:Polybrominated Biphenyls / Q000097:blood / Q000737:chemistry* / Q000302:isolation & purification; D052616:Solid Phase Extraction / Q000379:methods*
D055768:Halogenated Diphenyl Ethers; D006842:Hydrocarbons, Brominated; D011075:Polybrominated Biphenyls; C089796:hexabromocyclododecane; C020806:tetrabromobisphenol A
Hexabromocyclododecane; Human milk; Polybrominated diphenyl ethers; Serum samples; Tetrabromobisphenol A