真空冻干/快速溶剂萃取-气相色谱-质谱法测定土壤中35种不同种类半挥发性有机物  

Determination of 35 Different Types of Semi-volatile Organic Compounds in Soil by Vacuum Lyophilization and Rapid Solvent Extraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：邓云江[1] 邓昭祥 韩洁莲 杨健 钟蕾 杜作灵 张安丰 DENG Yunjiang;DENG Zhaoxiang;HAN Jielian;YANG Jian;ZHONG Lei;DU Zuoling;ZHANG Anfeng(Guizhou Central Laboratory of Geology and Mineral Resources,Guiyang 550018)

机构地区：[1]贵州省地质矿产中心实验室,贵州贵阳550018

出　　处：《分析科学学报》2024年第2期190-198,共9页Journal of Analytical Science

基　　金：贵州省地质矿产勘查开发局地质科研项目(黔地矿科合[2020]36号)。

摘　　要：建立了真空冻干/快速溶剂萃取-气相色谱-质谱法(GC-MS)测定土壤中35种不同种类半挥发性有机物(SVOCs)的方法。样品经真空冷冻脱水、快速溶剂萃取、旋转蒸发浓缩以及固相萃取SPE小柱净化后,氮吹定容,采用GC-MS上机测定。结果表明:土壤中35种SVOCs在10~1000μg/L范围内线性相关系数r^(2)≥0.991,方法检出限为0.034~0.40μg/kg,方法定量限为0.14~1.20μg/kg;以空白样品为基体进行加标回收实验,所得加标回收率为71.2%~113%,相对标准偏差(RSDs,n=7)为0.38%~13.3%,替代物荧蒽-D 10回收率为84.0%~92.5%;经实际样品检测验证,该方法灵敏、快速、准确可靠,适用于土壤中35种不同种类SVOCs的分析检测。Vacuum lyophilization and rapid solvent extraction coupled with gas chromatography-mass spectrometry(GC-MS)method was established for the determination of 35 different types of semi-volatile organic compounds(SVOCs)in soil.The sample was determined by GC-MS after vacuum freeze-dehydrating,rapid solvent extraction,rotary evaporation and SPE solid-phase extraction with nitrogen and diluted.The results showed that the correlation coefficients of 35 SVOCs in the range of 10.0-1000μg/L were above 0.991.The detection limits of the method ranged from 0.034 to 0.40μg/kg and lower limits of determination ranged from 0.14 to 1.20μg/kg.On the basis of blank sample,a test for recovery was made by standard addition method,values of recovery found were in the range of 71.2%-113%;and the recoveries of surrogate fluoranthene-D 10 were 84.0%-92.5%,with RSD(n=7)in the range of 0.38%-13.3%.The method is fast,simple and accurate,and fully meets the daily requirements for the detection of 35 SVOCs in the soil.

关 键 词：土壤 真空冻干 半挥发性有机物 快速溶剂萃取 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学]