快速溶剂-固相萃取法测定土壤中多溴联苯醚  

Determination of PBDEs in soil byhigh performance solvent extraction-solid phase extraction

作　　者：龚飞杰 齐安安 李一凡 张雄飞 黄琦 杨凌霄 GONG Feijie;QI Anan;LI Yifan;ZHANG Xiongfei;HUANG Qi;YANG Lingxiao(Environmental Research Institute,Shandong University,Qingdao 266237,Shandong,China;Jiangsu Collaborative Innovation Center for Climate Change,Nanjing 210023,Jiangsu,China)

机构地区：[1]山东大学环境研究院,山东青岛266237 [2]江苏省气候变化协同创新中心,江苏南京210023

出　　处：《山东大学学报(工学版)》2025年第1期149-156,共8页Journal of Shandong University(Engineering Science)

基　　金：青岛市自然科学基金资助项目(23-2-1-224-zyyd-jch)。

摘　　要：为建立快速、简便地分析土壤中12种多溴联苯醚(polybrominated diphenyl ethers,PBDEs)质量分数的检测方法,对仪器的参数和样品净化过程进行了优化。通过对比不同仪器参数组合、固相萃取柱种类、活化和洗脱溶剂组合及溶剂洗脱量对样品中12种PBDEs回收率的影响,确定了最优条件。在最优条件下,对实际土样进行加标验证,12种PBDEs的平均加标回收率为90.36%~121.40%,回收率相对标准偏差为4.11%~8.76%,东营油田土壤中PBDEs的质量分数为6.68×10^(-9)~105.68×10^(-9)。本方法使用C18固相萃取柱替代传统复合硅胶柱,简化了样品处理过程,具备操作便捷、稳定性好的优点,适用于大规模土壤样品中PBDEs的检测。In order to establish a rapid and convenient method to analyze the mass proportion of 12 polybrominated diphenyl ethers(PBDEs)in soil,the parameters of the analyzer and the sample purification process were optimized.By comparing the impact of different instrumental parameter combinations,different solid-phase extraction columns,different activation,and elution solvent systems,and elution solvent volumes on the recovery of 12 PBDEs,the optimal conditions were determined.Under optimal conditions,the average recovery of 12 PBDEs ranged from 90.36%to 121.40%,and the relative standard deviations of 12 PBDEs recovery ranged from 4.11%to 8.76%.The mass proportion of PBDEs in the soil samples of the Dongying oilfield ranged from 6.68×10^(-9)to 105.68×10^(-9).This method employed a C18 solid phase extraction column to replace the traditional composite silica gel column,having the advantages of simple pretreatment and acceptable stability,and making it suitable for large scale detecting of PBDEs in soil.

关 键 词：快速溶剂萃取 多溴联苯醚 土壤 气相色谱-质谱法 固相萃取 

分 类 号：X513[环境科学与工程—环境工程]