加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃
Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography
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摘要:
建立了加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤样品中16种多环芳烃（PAHs）的方法.旋蒸定容有效减少了污染物的引入，特别是萘、菲.研究了影响PAHs回收率的主要因素.优化后的条件为：萃取温度110℃，静态萃取时间3 min，冲洗量30%，氮气吹扫时间30 s，正己烷/丙酮（体积比2：1）为萃取液，1次静态萃取循环，弗罗里硅土柱为固相萃取小柱，正己烷/二氯甲烷（体积比7：3）为淋洗液，淋洗液体积10 mL.在20-200 mg·L-1范围内，各目标物线性关系（R2）为0.9994-1.目标物的检出限和定量限分别为0.08-2.50 mg·kg-1和0.25-8.33 mg·kg-1.在优化的实验条件下，加标水平为25 mg·kg-1和100 mg·kg-1时，目标物平均加标回收率分别为73.9%-105%、79.0%-110%，相对标准偏差（n=7）均小于10%.土壤PAHs QC样品的检测中，各目标物检测值均在参考值范围内；土壤PAHs QC样品加标回收率为63.4%-94.8%，适合实际土壤样品中多环芳烃的检测.
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关键词:
- 加速溶剂萃取 /
- 旋蒸定容 /
- 高效液相色谱 /
- 土壤 /
- 多环芳烃(PAHs)
Abstract:A method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in soil by high performance liquid chromatography was proposed based on accelerated solvent extraction and rotary evaporation to obtain a constant volume. The introduction of pollutants, especially for naphthalene and phenanthrene, could be effectively reduced by rotary evaporation to obtain a constant volume. The main factors affecting the recoveries of PAHs were investigated. Optimized conditions are:110℃ extraction temperature, three minutes static extraction, 30% rinse volume, 30 s nitrogen purge, a mixture of hexane and acetone (2:1, V/V) for extraction solvent, one static extraction cycle, florisil was used as SPE column, mixture of hexane and dichloromethane (7:3, V/V) as eluent, and 10 mL eluent volume. The correlation coefficients (R2) for PAHs were between 0.9994 and 1 in the range of 20-200 mg·L-1.The limits of detection and quantitation of PAHs were 0.08-2.50 mg·kg-1 and 0.25-8.33 mg·kg-1, respectively. Under the optimized experimental conditions, the recoveries of PAHs, with 25 mg·kg-1and 100 mg·kg-1 standard addition, were in the range of 73.9%-105% and 79.0%-110%, respectively, while the relative standard deviations (n=7) was less than 10%. In the detection of PAHs in soil QC sample, the concentrations of all the values of target analytes were within the reference value ranges and the recoveries were 63.4%-94.8%. Therefore, the present protocol is satisfactory for the detection of PAHs in actual soil samples.
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