快速溶剂(ASE)提取、凝胶渗透色谱(GPC)联合固相萃取(SPE)净化,高效液相色谱法测定土壤中的多环芳烃  

DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN SOIL BY ASE-GPC-SPE PURIFICATION AND HPLC DETECTION

作　　者：张茜[1] 刘潇威[1] 罗铭[1] 王璐[1] 李红[1] 王迪[1] 徐亚平[1] 

机构地区：[1]农业部环境保护科研监测所,天津300191

出　　处：《环境化学》2011年第4期771-777,共7页Environmental Chemistry

基　　金：中央级公益性科研院所基本科研业务费专项资金(农业部环境保护科研监测所)资助项目

摘　　要：建立了采用快速溶剂提取(ASE),固相萃取(SPE)与凝胶渗透色谱(GPC)协同净化方法,使用高效液相色谱-紫外-荧光检测器(HPLC-UV-FLD)串联检测土壤中多环芳烃类化合物多残留的检测方法.通过对加速溶剂提取仪提取条件,凝胶渗透色谱和固相萃取净化条件的优化,确定土壤中多环芳烃类化合物多残留的前处理方法:提取溶剂为丙酮∶二氯甲烷(V∶V,50∶50),提取温度120℃,GPC在线浓缩系统真空腔真空度为130mbr/140mbr,弗罗里硅土固相萃取柱净化,5mL二氯甲烷作为洗脱剂.方法回收率在62.9%—118.9%之间,RSD为0.6%—19.9%.A new method using ASE combined with solid-phase extraction and GPC cleanup followed by HPLC-tandem UV and fluorescence detection has been established for the quantitative determination of 16 PAHs in soils.In the method,the samples were extracted by ASE with acetone：dichloromethane（V∶V,50∶50）at 120 ℃,and dissolved in 9 mL hexane∶ethyl acetate（V∶V,50∶50）after taking the extract to dryness with evaporation at 25 ℃.Then the extract was injected into GPC column with hexane∶ethyl acetate（V∶V,50∶50）as the mobile phase at a flow rate of 5 mL·min-1 and GPC vacuum was 130 mbr/140 mbr.The 1340—3380 s fraction was collected for subsequent analysis.The portions collected from GPC were dissolved in 2 mL dichloromethane after taking the extract to dryness with nitrogen gas.Then the 2 mL extractions were purified by SPE using Florisil cartridges,eluted with 5 mL dichloromethane.Finally,the extraction was collected from SPE and dissolved in acetonitrile after taking it to dryness with nitrogen gas.The correlation coefficient of each PAH was r20.99,the recovery fell within 62.9%—118.9%,and the relative standard derivation of PAHs was between 0.6% and 19.9%.

关 键 词：多环芳烃 加速溶剂萃取 凝胶渗透色谱 固相萃取 高效液相色谱 

分 类 号：X833[环境科学与工程—环境工程]