【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%.更多还原

【Abstract】 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 r2>0.99,the recovery fell within 62.9%—118.9%,and the relative standard derivation of PAHs was between 0.6% and 19.9%.更多还原