摘要
本研究建立了同时提取、同时净化、同时测定土壤中多氯联苯、多溴二苯醚和多环芳烃等多种类持久性有机污染物(persistent organic pollutants,POPs)的方法,其提取和净化的最佳条件为:以V(丙酮)∶V(正己烷)=1∶1的混合溶液作为提取溶剂,超声提取3次;净化小柱为弗罗里硅土固相萃取柱;以V(正己烷)∶V(二氯甲烷)=9∶1的混合溶液作为洗脱溶剂,用量12 mL。经氮吹浓缩后,利用气相色谱-质谱联用法测定,内标法定量。结果表明:除2,2′,3,3′,4,4′,5,5′,6,6′-十溴二苯醚(BDE209)外,其余41种POPs仅在23.83 min内就得到很好的分离。42种目标POPs均在20~1000μg/L范围内线性关系良好,决定系数(R2)为0.9975~0.9999;方法的检出限为0.04~1.19 ng/g,加标回收率为71.04%~120.89%,相对标准偏差为0.88%~6.29%,日内重复性和日间重现性变化均小于11%。该方法大大减少了检测时间和工作量,并且操作简单、准确性好、灵敏度高,可大规模应用于废旧电器拆解场地等的土壤样品中POPs的测定分析,对POPs的检测及其环境行为研究等具有重要意义。
A method for simultaneous extraction,purification,and determination of persistent organic pollutants(POPs)in soil,such as polychlorinated biphenyls,polybrominated diphenyl ethers,and polycyclic aromatic hydrocarbons,was developed in this study.The optimum conditions for extraction and purification were as follows:Soil samples were extracted ultrasonically three times with acetone/n-hexane(1∶1,by volume),followed by purification with Florisil solid-phase extraction column,and eluted by 12 mL of n-hexane/dichloromethane(9∶1,by volume)mixture solution.The eluant was concentrated by gentle N2 streams and finally quantified by gas chromatography-mass spectrometry(GC-MS)with PCB209 as the internal standard.Except for 2,2′,3,3′,4,4′,5,5′,6,6′-decabromodiphenyl ether(BDE209),the other 41 POPs were efficiently separated within 23.83 min.Excellent linearity was observed in the concentration range of 20-1000μg/L for all POPs with the coefficients of determination(R2)of 0.9975-0.9999.The detection limits of 42 POPs were 0.04-1.19 ng/g,and the spiked recoveries ranged from 71.04%to 120.89%with relative standard deviations of 0.88%-6.29%,and intra-and inter-day reproducibility variations were less than 11%.In conclusion,this method greatly reduces time and workload and is characterized by simple operation,good accuracy,and high sensitivity.It can be widely applied to the determination and analysis of POPs in soil,such as e-waste disposal site soil,which will facilitate further studies on the fate and risk assessment of POPs.
作者
张浩
黄荣浪
陈旻彦
姜俊
杨澜
陈謇
吕志江
廖敏
汪海珍
徐建明
ZHANG Hao;HUANG Ronglang;CHEN Minyan;JIANG Jun;YANG Lan;CHEN Jian;LÜZhijiang;LIAO Min;WANG Haizhen;XU Jianming(Zhejiang Provincial Key Laboratory of Agricultural Resources and Environment,College of Environmental and Resource Sciences,Zhejiang University,Hangzhou 310058,China;Hangzhou Service Quality Testing Technology Co.,Ltd.,Hangzhou 311300,China;Bureau of Agriculture and Rural Affairs and Water Resource of Wenling,Taizhou 317500,Zhejiang,China)
出处
《浙江大学学报（农业与生命科学版）》
CAS
CSCD
北大核心
2022年第3期336-350,共15页
Journal of Zhejiang University:Agriculture and Life Sciences
基金
国家重点研发计划课题(2019YFC1803704)
国家自然科学基金面上项目(41771344)。
关键词
多氯联苯
多溴二苯醚
多环芳烃
超声提取
固相萃取净化
气相色谱-质谱联用
polychlorinated biphenyls
polybrominated diphenyl ethers
polycyclic aromatic hydrocarbons
ultrasonic extract
solid phase extraction purification
gas chromatography-mass spectrometry
