加速溶剂萃取-气相色谱法测定土壤、植物样品中13种多溴联苯醚  

Determination of 13 polybrominated biphenyl ethers in soil and plant using accelerated solvent extraction and gas chromatography

作　　者：由宗政[1,2] 孔德洋[2] 许静[2] 何健[2] 裴佳佳[1] 付银杰[1] 单正军[1,2] 

机构地区：[1]南京农业大学资源与环境科学学院,南京210095 [2]环保部南京环境科学研究所,南京210042

出　　处：《环境化学》2013年第7期1410-1416,共7页Environmental Chemistry

基　　金：环保公益性行业科研专项(201009026)资助

摘　　要：采用气相色谱(GC-ECD)法,建立了土壤和植物样品中13种多溴联苯醚(PBDEs)的分析方法,以正己烷∶二氯甲烷(1∶1)作为萃取溶剂,样品经加速溶剂萃取仪(ASE)萃取、固相萃取净化后,使用气相色谱仪分析样品中的13种PBDEs.结果表明,所选取的13种多溴联苯醚(PBDEs)得到了较好的分离,且该方法中BDE-209在土壤和植物样品中的平均添加回收率分别为68.1%—75.1%和65.1%—72.1%,其余12种BDE的回收率分别为70.3%—106.9%、67.7%—93.4%;BDE-209方法检出限分别为0.26 ng.g-1、0.64 ng.g-1,其余12种BDE的方法检出限分别为0.016—0.043 ng.g-1、0.028—0.096 ng.g-1.本实验方法测定多组分PBDEs的灵敏度和准确度较高、稳定性和回收率良好,可满足于环境样品中PBDEs的分析.A method was developed for the determination of 13 polybrominated diphenyl ethers （PBDEs） in soil and plant samples by accelerated solvent extraction （ASE） combined with gas chromatography （GC/μECD）. The samples were extracted by ASE using n-hexane-dichloromethane （ V： V = 1 ： 1 ） as solvents. The extracts were cleaned with SPE before analysis with GC/μECD. The results show that all the selected PBDEs were well separated. The average recovery of BDE-209 was 68.1%-75.1% and 65.1%-72.1%, respectively, in soil and plant samples, while the values of the other PBDEs were in the range of 70.3%-106.9% and 70. 3%-93.4%, respectively. The detection limit of BDE-209 was 0.26 ng·g-1 and 0.64 ng·g-1 in soil and plant samples, respectively. Detection limits of the other 12 PBDEs were an order of magnitude lower, in the range of 0. 016-0.043 ng.g-land 0. 028-0. 096 ng·g-1 in soil and plant samples, respectively. Because of the high sensitivity and accuracy, good stability and recovery, this method is ready to be applied for the analysis of PBDEs in environmental samples.

关 键 词：多溴联苯醚 气相色谱 加速溶剂萃取 固相萃取 

分 类 号：X833[环境科学与工程—环境工程] O657.71[理学—分析化学]