快萃仪/GC-MS法测定土壤中11种半挥发性有机物

张安丰; 杨健; 邓昭祥; 钟蕾; 杜作灵; 邓云江; 石春兰; 张舟

张安丰,杨健,邓昭祥,钟蕾,杜作灵,邓云江,石春兰,张舟.快萃仪/GC-MS法测定土壤中11种半挥发性有机物[J].贵州地质,2020,37(4):551-557

快萃仪/GC-MS法测定土壤中11种半挥发性有机物

Rapid Determination of 11 SVOCs in Soil by Accelerated Solvent Extraction/GC-MS

投稿时间：2020-04-28

DOI：

中文关键词: 快速溶剂萃取气相色谱-质谱法土壤 SVOCs

英文关键词:Accelerated solvent extraction GC-MS Soil SVOCs

基金项目:贵州省地质矿产勘查开发局地质科研项目，土壤中不同种类半挥发性有机污染物检测方法优化及其应用研究(黔地矿科合〔2020〕36号)。

作者	单位
张安丰	贵州省地质矿产中心实验室，贵州贵阳550018
杨健	贵州省地质矿产中心实验室，贵州贵阳550018
邓昭祥	贵州省地质矿产中心实验室，贵州贵阳550018
钟蕾	贵州省地质矿产中心实验室，贵州贵阳550018
杜作灵	贵州省地质矿产中心实验室，贵州贵阳550018
邓云江	贵州省地质矿产中心实验室，贵州贵阳550018
石春兰	贵州省地质矿产中心实验室，贵州贵阳550018
张舟	贵州省地质矿产中心实验室，贵州贵阳550018

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中文摘要:

本文建立了快速溶剂萃取仪(Buchi 瑞士)-气相色谱-质谱仪(GC-MS)测定土壤中11种半挥发性有机物(SVOCs)含量的方法。土壤样品经正己烷-丙酮(1∶1)快速溶剂萃取，换相浓缩后，利用硅酸镁小柱进行净化，直接进GC-MS测定。结果表明，在100 μgL-11 000 μg·L-1浓度范围内，11种半挥发性有机物(SVOCs)的线性相关系数≥0995以上，平均响应因子RFRSD≤980，方法的检出限为0000 4 mg·kg-10000 8 mg·kg-1，测定下限为0001 6 mg·kg-10003 3 mg·kg-1。以空白样品为基体进行加标回收试验，所得回收率为746%1024%，替代物荧蒽-D10回收率为800%920%，测定值的相对标准偏差(n=7)在224%102%之间。该方法灵敏、快速、准确可靠，完全满足实验室对实际土壤中11种半挥发性有机物(SVOCs)的检测要求，可为土壤中11种半挥发性有机物(SVOCs)的污染情况提供快速检测依据。

英文摘要:

An analytical method for the determination of 11 Semi-volatile organic compounds (SVOCs) in soil by accelerated solvent extraction (Buchi Switzerland) coupled with gas chromatography-mass spectrometry (GC-MS) was developed. The soil samples were quickly extracted with n-hexane and acetone(1∶1), and the extract was concentrated by phase conversion, then purified by magnesium silicate column. The samples were directly subjected to GC-MS after dewater. The results showed that the correlation coefficients of 11 SVOCs were above 0.995 in the range of 10.0 μg·L-11 000 μg·L-1, RF RSD＜9.80%. The detection limits of the method found were ranged from 0.000 4 to 0.000 8 mg·kg-1 and lower limits of determination found were ranged from 0.001 6 to 0.003 3 mg·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 74.6%102.4%; and the recoveries of surrogate fluoranthene-D10 were 80.0%92.0%, with RSD’s (n=7) in the range of 2.24%10.2%. The method is fast, simple and accurate, and fully meets the daily requirements for the detection of 11 SVOCs in the soil, and can provide a rapid detection basis for soil pollutants.

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