气相色谱–质谱法连续测定土壤中的多环芳烃和有机氯农药

Continuous Determination of Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in Soil by GC-MC

摘要: 建立同时测定土壤样品中18种有机氯农药和16种多环芳烃的快速溶剂萃取——气相色谱/质谱方法，对前处理过程中的快速溶剂萃取以及净化步骤进行优化，并优化气相色谱–质谱仪仪器参数。优化后测定时间较短，目标物质分离效果良好。方法线性范围内线性相关系数0.9955~0.9998，方法检出限为1.1 g/kg~3.2 g/kg，测定低浓度(10 ppb)空白加标、中等浓度(100 ppb)基体加标、高浓度(500 ppb)基体加标相对标准偏差(n = 7)分别为2.8%~27.0%、1.6%~8.2%、07%~12.2%，加标回收率分别为60.4%~128.9%、60.4%~126.7%、60.4%~125.5%，证明该方法提取效果好，精密度和准确度较高，可以用于同时检测土壤中的多环芳烃和有机氯农药。

Abstract: A gas chromatographymass spectrometry method coupled with accelerated solvent extraction (ASE) was established for the continuous determination of 18 organochlorine pesticides (OCPs) and 16 Polycyclic Aromatic Hydrocarbons(PAHs) in soil samples. After optimizing the rapid solvent extraction and purification steps during pretreatment, and the parameters of gas chromatography-mass spectrometer, the measurement time is relatively short, and the separation effect of the target material is good. The test results showed that the linear correlation coefficient in the linear range of the method was from 0.9955 to 0.9998, and the detection limit of the method was between 1.1 g/kg and 3.2 g/kg. The relative standard deviations (n = 7) of low concentration (10 ppb) blank labeling, medium concentration (100 ppb) matrix labeling, and high concentration (500 ppb) matrix labeling (n=7) were 2.8%~27.0%, 1.6%~8.2% and 07%~12.2%, respectively, The recovery rate of the target matrix were 60.4%~128.9%, 60.4%~126.7% and 60.4%~125.5%, respectively, which proved that this method had good extraction effect, high precision and accuracy, and indicated that this method could simultaneously detect PAHs and OCPs in soil.