title: Simple and fast analysis of tetrabromobisphenol A, hexabromocyclododecane isomers, and polybrominated diphenyl ethers in serum using solid-phase extraction or QuEChERS extraction followed by tandem mass spectrometry coupled to HPLC and GC.
abstract: Two simplified sample preparation procedures for simultaneous extraction and clean-up of tetrabromobisphenol A, α-, β-, and γ-hexabromocyclododecane and polybrominated diphenyl ethers in human serum were developed and validated. The first procedure was based on solid-phase extraction. Sample extraction, purification, and lipid removal were carried out directly on an Oasis HLB cartridge. The second procedure was a quick, easy, cheap, effective, rugged, and safe-based approach using octadecyl-modified silica particles as a sorbent. After sample extraction and cleanup, tetrabromobisphenol A/hexabromocyclododecane was separated from polybrominated diphenyl ethers by using a Si-based cartridge. Tetrabromobisphenol A and hexabromocyclododecane were then detected by high-performance liquid chromatography coupled to tandem mass spectrometry, while polybrominated diphenyl ethers were detected by gas chromatography coupled to tandem mass spectrometry. The results of the spike recovery test using fetal bovine serum showed that the average recoveries of the analytes ranged from 87.3 to 115.3% with relative standard deviations equal to or lower than 13.4 %. Limits of detection of the analytes were in the range of 0.4-19 pg/mL except for decabromodiphenyl ether. The developed method was successfully applied to routine analysis of human serum samples from occupational workers and the general population. Extremely high serum polybrominated diphenyl ethers levels up to 3.32 × 104ng/g lipid weight were found in occupational workers.
authors.affiliation: School of Public Health and Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
authors.forename: Jian
authors.initials: J
authors.lastname: Li
authors.affiliation: School of Public Health and Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
authors.forename: Tian
authors.initials: T
authors.lastname: Chen
authors.affiliation: School of Public Health and Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
authors.forename: Yuwei
authors.initials: Y
authors.lastname: Wang
authors.affiliation: School of Public Health and Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
authors.forename: Zhixiong
authors.initials: Z
authors.lastname: Shi
authors.affiliation: School of Public Health and Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
authors.forename: Xianqing
authors.initials: X
authors.lastname: Zhou
authors.affiliation: School of Public Health and Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
authors.forename: Zhiwei
authors.initials: Z
authors.lastname: Sun
authors.affiliation: Shandong Center for Disease Control and Prevention, Jinan, Shandong, China.
authors.forename: Dejun
authors.initials: D
authors.lastname: Wang
authors.affiliation: China National Center for Food Safety Risk Assessment, Beijing, China.
authors.forename: Yongning
authors.initials: Y
authors.lastname: Wu
mesh_terms: D001774:Blood Chemical Analysis / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D004785:Environmental Pollutants / Q000097:blood; D008401:Gas Chromatography-Mass Spectrometry; D055768:Halogenated Diphenyl Ethers / Q000097:blood; D006801:Humans; D006838:Hydrocarbons / Q000097:blood*; D006842:Hydrocarbons, Brominated / Q000097:blood; D057230:Limit of Detection; D016273:Occupational Exposure; D011075:Polybrominated Biphenyls / Q000097:blood; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry
chemical_list: D004785:Environmental Pollutants; D055768:Halogenated Diphenyl Ethers; D006838:Hydrocarbons; D006842:Hydrocarbons, Brominated; D011075:Polybrominated Biphenyls; C089796:hexabromocyclododecane; C020806:tetrabromobisphenol A
keywords: dispersive solid-phase extraction; hexabromocyclododecane; polybrominated diphenyl ethers; serum; tetrabromobisphenol A