Concurrent extraction,clean‐up,and analysis of polybrominated diphenyl ethers,hexabromocyclododecane isomers,and tetrabromobisphenol A in human milk and serum |
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Authors: | Zhixiong Shi Yifei Wang Piye Niu Jiandi Wang Zhiwei Sun Shuhua Zhang Yongning Wu |
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Institution: | 1. School of Public Health, Capital Medical University, , Beijing, China;2. Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, , Beijing, China;3. Maternal and Child Health Care Hospital of Shunyi District, , Beijing, China;4. China National Centre for Food Safety Risk Assessment, , Beijing, China |
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Abstract: | 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. |
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Keywords: | Hexabromocyclododecane Human milk Polybrominated diphenyl ethers Serum samples Tetrabromobisphenol A |
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