School of Public Health, Capital Medical University, Beijing, China; Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, China.
J Sep Sci. 2013 Oct;36(20):3402-10. doi: 10.1002/jssc.201300579. Epub 2013 Sep 1.
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.
已开发并验证了一种同时提取、净化和分析人乳和血清中多溴二苯醚 (PBDEs)、α-、β-和 γ-六溴环十二烷 (HBCD) 和四溴双酚 A (TBBPA) 的方法。分别使用丙酮/正己烷 1:1（v/v）和甲基叔丁基醚/正己烷 1:1（v/v）进行加速溶剂萃取和液液萃取，从奶和血清样品中提取。通过凝胶渗透色谱和硫酸处理去除共提取的生物材料。使用 Supelco LC-Si SPE 小柱对 PBDEs 和 HBCD/TBBPA 进行分级。然后使用 GC-MS 检测 PBDEs，使用 UPLC-MS/MS 检测 HBCDs 和 TBBPA。优化了预处理程序，并通过 MS 或 MS/MS 研究了分析物的特征离子和碎裂。通过在 0.05-10 ng/g 浓度下进行基质加标测试进行回收率测试。回收率范围为 78.6-108.8%，RSD 等于或低于 14.04%。LODs 为 1.8-60 pg/g。通过分析实际人体样本测试了所开发方法的实用性，并检测和分析了不同样本中的几种溴化阻燃剂。
