气相色谱质谱法测定《全国土壤污染状况详查》项目中多环芳烃

Determination of polycyclic aromatic hydrocarbons in the national soil pollution survey with chromatography-mass spectrometry

建立加速溶剂萃取-固相柱净化-气相色谱-质谱法测定《全国土壤污染状况详查》项目中多环芳烃的方法。对加速溶剂萃取以及分析仪器的参数条件进行优化,考察了氮吹体积的影响,有效地保证16种多环芳烃较高的回收率。结果表明,16种多环芳烃在10~500μg/L范围内线性良好,该方法检出限在0.019~0.046 mg/kg之间。用新鲜土壤配置低、中、高加标水平分别为0.1,0.4,1.0 mg/kg的加标样品,16种多环芳烃的加标回收率在61.6%~115.6%之间,平行分析(n=6)得到的相对标准偏差(RSD)均小于19%,方法具有较高的准确度和精密度,利用生态环境部标样所提供的多环芳烃标准样品作为质控样,目标物质含量均在有效范围内。该方法能够为测定土壤中多环芳烃的含量提供技术支撑。

In this paper,a method for the determination of polycyclic aromatic hydrocarbons(PAHs)in the national soil pollution survey by accelerated solvent extraction-solid phase column purification-gas chromatography mass spectrometry was established.The parameters of accelerated solvent extraction and analytical instruments were optimized.The influence of nitrogen blowing volume was investigated,which effectively ensured the high recovery rate of 16 PAHs.The results showed that PAHs has good linearity in the range of 10-500μg/L,and the detection limit was 0.019-0.046 mg/kg.The spiked samples with low,medium and high spiked levels of 0.1,0.4,1.0 mg/kg were prepared with fresh soil.The spiked recoveries of PAHs were between 61.6%and 115.6%,and the parallel analysis(n=6)was obtained.The relative standard deviation(RSD)is less than 19%.The method has high accuracy and precision.The PAHs standard samples provided by the institute for environmental reference materials were used as quality control sample,and the contents of target substance were within the valid range.The method can provide technical support for the determination of PAHs in soil.