加速溶剂萃取-固相萃取净化-气相色谱/质谱法测定土壤中的多环芳烃

建立了加速溶剂萃取-固相萃取净化-气相色谱/质谱法同时测定土壤中16种多环芳烃的方法。土壤样品经正己烷-丙酮提取,经无水Na₂SO₄脱水、氮吹浓缩后,弗罗里土小柱净化,采用气相色谱/质谱检测,内标法定量。结果表明:该方法在质量浓度0.4～10μg/mL范围内线性良好,相关系数(r²)大于0.9962,检出限为4.8～25μg/kg,定量限为19.2～100μg/kg;在0.05,0.15,0.40 mg/kg 3个加标水平下的平均回收率为55.4%～129.0%,相对标准偏差为1.5%～11%。采用该方法检测土壤样品,除苊烯、苊、芴3种多环芳烃未检出外,其他13种多环芳烃均有检出,其含量范围在6.6～86μg/kg。

Determination of PAHs in soil by accelerated solvent extraction-solid phase extraction-gas chromatography/mass spectrometry

A method for the simultaneous determination of 16 polycyclic aromatic hydrocarbons(PAHs)in soil by ASE-SPE-GC/MS was established.The soil samples were extracted by n-hexane-acetone,dehydrated by anhydrous sodium sulfate and concentrated by nitrogen blowing,purified by florisil column,detected by gas chromatography-mass spectrometry and quantified by internal standard method.The results showed that the linearity of the method was good in the range of 0.4-10μg/mL,and the correlation coefficient(r²)was more than 0.9962 with the detection limit of 4.8-25μg/kg and the quantitative limit of 19.2-100μg/kg.The average recoveries at spiked levels of 0.05,0.15 and 0.40 mg/kg ranged from 55.4%to 129.0%with the relative standard deviations from 1.5%to 11%.In this method,13 PAHs were detected in the concentration range of 6.8-86μg/kg in a soil sample except acenaphthene,acenaphthene and fluorene.