摘要
采用索氏抽提、凝胶渗透色谱柱和多层硅胶氧化铝柱分离净化,并采用气相色谱质谱联用法定量分析了污泥中的多溴联苯醚(PBDEs),建立了城市污泥中PBDEs测定的质量控制和质量保证(QC/QA)措施。样品中所检测的19种目标物的回收率为82%~119%,回收率指示物BDE-50和BDE-172的回收率分别为108%±4.91%和99%±4.72%。三-七溴联苯醚(即BDE-17、28、33、47、49、66、99、100、138、153、154、183和190)的仪器检出限分别为0.55、0.46、0.52、0.33、0.36、O.22、0.14、0.33、0.24、0.10、0.14、0.27、1.5Pg;八~十溴联苯醚(即BDE-196、203、206、207、208和209)的仪器检出限分别为0.49、0.66、0.66、0.69、1.3和3.1pg。本方法具有较低的检出限和较高的回收率,重复性好,可用于城市污泥样品中多溴联苯醚的检测。
Soxhlet extraction method, gel permeation chromatography column, multilayer silica and alumina column and GC-MS were used for quantitative analysis of polybrominated diphenyl ethers (PBDEs) in sewage sludge. A method of quality control and quality assurance (QC/QA) for the determination of PBDEs was developed. The recoveries for all 19 targets are 82% to 119% , and the recover- ies of surrogates (BDE-50 and BDE-172) are ( 108 ±4.91 ) % and (99 ±4.72) % respectively. The instrumental detection limits for tri- to hepta-BDEs (namely BDE-17, 28, 33, 47,49, 66, 99, 100, 138, 153, 154, 183 and 190) are 0.55,0.46, 0.52, 0.33,0.36, 0.22, 0. 14, 0.33,0.24, 0. 10, 0.14, 0.27, and 1.5 pg respectively, and those for octato deca-BDEs (namely BDE-196, 203, 206, 207, 208 and 209) are 0.49, 0.66, 0.66, 0.69, 1.3 and 3.1 pg respectively. Based on the low method detection limits, satisfactory recoveries and good reproducibility, this method is suitable for determination of PBDEs in sludge samples from wastewater treatment plants.
出处
《中国给水排水》
CAS
CSCD
北大核心
2011年第6期90-93,共4页
China Water & Wastewater
基金
国家自然科学基金资助项目(40901251/D010901)
污染控制与资源化研究国家重点实验室自主研究课题(PCRRY09001)