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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