加速溶剂萃取-固相萃取-层析柱净化法同时测定沉积物中多氯联苯、多溴二苯醚和有机磷阻燃剂  

Simultaneous Determination of Polychlorinated Biphenyls,Polybrominated Diphenyl Ethers and OrganophosphateFlame Retardants in Sediments Using Accelerated SolventExtraction-Column Purification-Solid Phase Extraction method

作　　者：张玮庭 宋善军 卢柏灵 彭子娟 李彭辉[1] ZHANG Wei-Ting;SONG Shan-Jun;LU Bo-Ling;PENG Zi-Juan;LI Peng-Hui(Tianjin University of Technology,Tianjin 300384,China;National Institute of Metrology,Beijing 100029,China)

机构地区：[1]天津理工大学,天津300384 [2]中国计量科学研究院,北京100029

出　　处：《分析化学》2021年第4期571-580,共10页Chinese Journal of Analytical Chemistry

基　　金：中国计量科学研究院基本科研业务费(No.AKY1720);天津市重点研发计划科技支撑重点项目(No.18YFZCSF01400);天津市高等学校科技发展基金计划项目(No.2017KJ244)资助。

摘　　要：建立并优化了对沉积物中多氯联苯(PCBs)、多溴联苯醚(PBDEs)和有机磷酸酯阻燃剂(OPFRs)3种有机污染物同时测定的分析方法。采用加速溶剂萃取(ASE)法对沉积物样品进行萃取,并通过固相萃取与层析柱串联方法对样品进行净化。在优化的分析条件下,PCBs的平均加标回收率为104.1%~121.7%,PBDEs的平均加标回收率为80.7%~101.6%,OPFRs的平均加标回收率为80.7%~132.2%,本方法可有效降低基质效应的影响。应用标准物质SRM-1944进行方法确证,证明本方法准确性良好。对采集于黄河三角洲地区的20个表层沉积物样品进行分析,分别检出了PBDEs和OPFRs等12种化合物,浓度范围为0.01~0.38 ng/g和1.18~21.99 ng/g,该区域有机磷系阻燃剂含量明显高于溴代阻燃剂。实际样品分析结果表明,本方法可满足实际样品分析检测的需求。An analytical method for simultaneous determination of three organic pollutants,including polychlorinated biphenyls(PCBs),polybrominated diphenyl ethers(PBDEs)and organic phosphorus flame retardants(OPFRs),in sediments was developed.Accelerated solvent extraction(ASE)was used to extract the targets from sediment samples,and the extracts were purified by solid phase extraction coupled with chromatography column purification.After optimization of the reaction conditions,the recoveries were 104.1%-121.7%for PCBs,80.7%-101.6%for PBDEs,and 80.7%-132.2%for OPFRs.The developed method effectively eliminated the matrix effects.The method was verified by SRM-1944,showing satisfying accuracy.The method was further applied to detection of 20 surface sediment samples collected from the Yellow River Delta,and 12 compounds including PBDEs and OPFRs were detected with the concentration ranges of 0.01-0.38 ng/g and 1.18-21.99 ng/g.The results showed that the content of organophosphorus flameretardants in this area was higher than that of brominated flame retardants,and the method could be used for the detection of real samples.

关 键 词：多氯联苯 多溴联苯醚 有机磷酸酯 沉积物 同时测定 

分 类 号：X832[环境科学与工程—环境工程] O658.2[理学—分析化学]