Sánchez-Brunete Consuelo, Miguel Ester, Tadeo José L
Departamento de Medio Ambiente, INIA, Madrid, Spain.
J Sep Sci. 2009 Jan;32(1):109-17. doi: 10.1002/jssc.200800479.
A method for the determination of 14 polybrominated diphenyl ethers (PBDEs) in sludge from wastewater treatment plants is presented. PBDEs were extracted by matrix solid-phase dispersion assisted by sonication and determined by isotope dilution gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode, using labelled( 13)C-PBDEs as internal standards. The limits of detection and quantification for the tri- to hepta-BDEs were in the range of 0.05 to 0.5 ng/g dry weight and 0.15 to 1.8 ng/g dry weight, respectively, and 1.6 ng/g dry weight and 5.6 ng/g dry weight for deca-BDE-209. The proposed analytical method was applied to determine PBDE levels in sewage sludge samples collected from 19 water treatment plants located in the province of Madrid (Spain). In all of the examined samples, BDE-100 and BDE-154 were the main compounds found with a mean concentration of 3.9 and 2.0 ng/g, respectively. PBDEs were detected in all of the samples, and their total concentrations not considering BDE-209 were between 3.9 and 23.0 ng/g dry weight. The dominant PBDE congener in sewage sludge was BDE-209, which constituted 38.7 to 97.3% of the total, and showed concentration levels ranging from 8.1 to 717.2 ng/g dry weight.
本文提出了一种测定污水处理厂污泥中14种多溴二苯醚（PBDEs）的方法。采用超声辅助基质固相分散萃取PBDEs，以标记的（13）C-PBDEs为内标，在选择离子监测模式下，通过同位素稀释气相色谱-电子轰击质谱检测法进行测定。三至七溴二苯醚的检测限和定量限分别在0.05至0.5 ng/g干重和0.15至1.8 ng/g干重范围内，十溴二苯醚-209的检测限和定量限分别为1.6 ng/g干重和5.6 ng/g干重。将所提出的分析方法应用于测定从西班牙马德里省19个水处理厂采集的污水污泥样品中的PBDEs水平。在所有检测样品中，BDE-100和BDE-154是主要检出化合物，平均浓度分别为3.9 ng/g和2.0 ng/g。所有样品中均检测到PBDEs，不考虑BDE-209时，其总浓度在3.9至23.0 ng/g干重之间。污水污泥中占主导地位的PBDE同系物是BDE-209，占总量的38.7%至97.3%，浓度水平在8.1至717.2 ng/g干重之间。
