气相色谱-质谱法快速检测土壤中16种多环芳烃
Rapid determination of 16 polycyclic aromatic hydrocarbons in soil by gas chromatography-mass spectrometry
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摘要: 本文利用一种新型的10 m气相色谱柱结合气相色谱-质谱联用仪测定了土壤中16种多环芳烃、5种氘代内标及2种替代物，10 min内即可完成分析.采用环境行业标准推荐的加压流体萃取方法提取土壤中的多环芳烃.所获得的萃取液经GCMS分析，快速法色谱图与常规法的色谱图相似，但响应更高，快速柱上16种多环芳烃在5.0-400 μg·L-1范围内线性关系良好，r ≥ 0.997，检出限范围为0.04-0.38 μg·kg-1，定量限为0.16-1.52 μg·kg-1.在低、中、高的浓度加标水平下，精密度范围为5.1%-21.2%，准确度范围为45.1%-91.3%.数据比较显示，两种色谱柱都符合环境标准分析方法要求，但快速测定对于大批量样品分析具有显著优势，既可提高效率又可节约成本.Abstract: In this paper, a new 10 m short column of gas chromatograph combined with the gas chromatograph-mass spectrometer (GC/MS) was used to determine 16 polycyclic aromatic hydrocarbon(PAHs), 5 deuterium internal standard and 2 substitutes in soil. The analysis could be completed within 10 minutes. Using the accelerated solvent extraction method provided by the environmental industry standard, the obtained extraction solution was analyzed by GC/MS. Under the optimal conditions, the chromatogram of the fast method was similar to that of the conventional column, however, the response was higher. The 16 PAHs have a good linear relationship in the range of 5.0-400 μg·L-1, r ≥ 0.997, and detection limit range is 0.04 -0.38 μg·kg-1, minimum quantitative detection limit is 0.16 -1.52 μg·kg-1. The precision ranges from 5.1% to 21.2% and the accuracy ranges from 45.1% to 91.3% at the three concentration levels. Results show that both the two columns the requirements of the environmental standard analytical method. However, the rapid method has significant advantages in the analysis of large quantities of samples, which can improve the efficiency and save the cost.
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