气相色谱质谱法测定土壤中16种多环芳烃

Determination of 16 polycyclic aromatic hydrocarbons in soil by gas chromatography/mass spectrometry

本文研究加速溶剂萃取、固相萃取小柱净化、气相色谱-质谱法测定土壤中16种多环芳烃的分析方法,选择用丙酮/正己烷(1:1,v:v)作为提取溶液,提取液经旋蒸,置换溶剂后,经固相萃取小柱净化后,用二氯甲烷/正己烷(2:1,v:v)进行洗脱,洗脱液浓缩,加入内标后,定容至1.0mL,用气相色谱-质谱仪进行测定。结果表明,16种PAHs在10-1000μg/L浓度范围内线性良好,平均相对响应因子RSD%<20%,16种PAHs的方法检出限为0.10-0.32μg/kg,完全符合土壤样品中PAHs分析的质量控制要求。该方法快速、准确、稳定,适用于土壤中16种PAHs的准确测定。

The analytical methods for the determination of 16 polycyclic aromatic hydrocarbons in soil by accelerated solvent extraction, solid phase extraction cartridge purification and gas chromatography-mass spectrometry were studied. The acetone/n-hexane (1:1, v:v) was selected as the extraction solution. The extract is subjected to rotary distillation, and the solvent is replaced. After purification by a solid phase extraction cartridge, the mixture is eluted with dichloromethane/n-hexane (2:1, v:v), and the eluent is concentrated. After the internal standard is added, The volume was adjusted to 1.0 mL and measured by gas chromatography-mass spectrometry. The results showed that 16 PAHs had good linearity in the concentration range of 10-1000 μg/L, and the average relative response factor RSD%< 20 %. The detection limit of 16 PAHs was 0.10-0.32 μg/kg, which was compliance with soil samples of quality control requirements for PAHs analysis. The method is fast, accurate and stable, and is suitable for accurate determination of 16 kinds of PAHs in soil.