快速溶剂萃取-气相色谱-质谱法测定土壤中24种半挥发性有机物含量  

GC-MS Determination of 24 Semi-Volatile Organic Compounds in Soil with Accelerated Solvent Extraction

作　　者：梁焱[1] 陈盛[1] 张鸣珊[1] 李腾崖[1] 何书海[1] 

机构地区：[1]海南省环境监测中心站,海口571126

出　　处：《理化检验（化学分册）》2016年第6期677-683,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：采用快速溶剂萃取-气相色谱-质谱法测定土壤中24种半挥发性有机物的含量。土壤样品以正己烷-乙酸乙酯(5+1)混合液进行萃取,所得萃取物用弗罗里硅土固相萃取小柱净化。在气相色谱分离中用DB-5MS色谱柱为固定相,在质谱分析中采用选择离子监测模式。24种半挥发性有机物在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限在0.83~4.48μg·kg^(-1)之间,测定下限在3.32~15.8μg·kg^(-1)之间。以空白样品为基体进行加标回收试验,所得回收率在60.4%~123%之间。测定值的相对标准偏差(n=4)在5.2%~19%之间。GC-MS was applied to the determination of 24 semi-volatile organic compounds in soil with accelerated solvent extraction. The soil sample was extracted with a mixture of hexane and ethyl acetate （5＋1） and the extract was then purified on Florisil solid phase extraction column. DP-5MS chromatographic column was used for GC separation and selected ion monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass concentration of the 24 semi-volatile organic compounds were kept in definite ranges. Detection limits of the method found were ranged from 0. 83 to 4. 48 μg·kg^ 1 and lower limits of determination found were ranged from 3. 32 to 15. 8 μg·kg^-1. On the basis of blank sample, test for recovery was made by standard addition method, values of recovery found were in the range of 60.4%-123%, with RSD＇s （n=4） in the range of 5.2 %- 1 9 %.

关 键 词：气相色谱-质谱法 土壤 半挥发性有机物 快速溶剂萃取 

分 类 号：O657.63[理学—分析化学]