气相色谱-质谱联用检测土壤中16种多环芳烃的方法研究

Study on the Method of Analyzing 16 Polycyclic Aromatic Hydrocarbons in Soil by Gas Chromatography-Mass Spectrometry

实验建立了气相色谱质谱(GC-MS)联用检测土壤中16种多环芳烃的方法。采用正己烷和丙酮混合溶液超声萃取、离心浓缩、硅胶层析柱净化的前处理方法和气相色谱分离、质谱检测的仪器分析手段,对土壤样品进行了PAHs的定性与定量分析。结果显示,在浓度为0.3~6 mg/L范围内PAHs校准曲线线性关系良好,r2高于0.99,标准偏差低于20%;浓度为5~100μg/kg范围内目标物的加标回收率为51%~111%,相对标准偏差小于20%;实验方法确定的PAHs的最低检测限为3.86~9.26μg/kg;实际5个土壤样品检测各化合物浓度范围为0.31~21.64μg/kg,重复检测的标准差在0.16~2.54μg/kg范围内。结果表明,设计的PAHs实验方法可靠,满足土壤样品PAHs方法检测要求。

A method for the determination of 16 polycyclic aromatic hydrocarbons in soil by gas chromatography-mass spectrometry was established.The experiment used the pre-treated method included ultrasonic extraction of n-hexane and acetone mixed solution,centrifugation and concentration,purification of silica gel column,and used the gas chromatography to separate,and mass spectrometry to detect in the qualitative and quantitative analysis process.The experimental results show that the calibration curve of PAHs in the range of 0.3~6 mg/L has a good linear relationship,and that all of r 2 values are above 0.99,and the quasi-bias of the repeated test is less than 20%;the spiked recovery of the target in the range of 5~100μg/kg is 51~111%,and the relative standard deviation is less than 20%;the minimum detection line(MDL)of PAHs by this experimental method is 3.86~9.26μg/kg;the standard deviation of the actual 5 soil samples is in the range of 0.16~2.54μg/kg.The test results show that the PAHs experimental method designed by our laboratory is reliable and meets the requirements of PAHs method test for soil samples.