加速溶剂萃取-串联质谱法测定土壤中8种有机氯农药和16种多环芳烃

Determination of 8 Organochlorine Pesticides and 16 Polycyclic Aromatic Hydrocarbons in Soil Using Gas Chromatography-tandem Mass Spectrometry Combined with Accelerated Solvent Extraction

建立了加速溶剂提取(ASE)-Florisil柱净化-三重四级杆串联质谱(GC-MS/MS)同时分析土壤中8种有机氯农药(OPCs)和16种多环芳烃(PAHs)的方法。优化了GC-MS/MS分析参数和Florisil柱净化条件,并将其应用于实际土壤样品的分析。结果表明:方法在2.0~50μg/L范围内线性良好,相关系数均>0.990,各目标化合物的方法检出限为0.01~0.22μg/kg。空白硅藻土样品的加标回收率在71.2%~118%之间,7次平行测定的RSD为1.9%~7.3%。用该方法测定徐州某地6个农村土壤样品,OPCs和PAHs均有检出,其中OPCs的质量分数在2.9~5.0μg/kg之间,PAHs的质量分数在10.2~20.3μg/kg之间。

An effective method was developed and applied to determine 8 kinds of organochlorine pesticides （OPCs） and 16 kinds of polycyclic aromatic hydrocarbons （PAHs） in soil using gas chromatography-tandem mass spectrometry combined with accelerated solvent extraction. The GC-MS/MS parameters and Florisil column purification conditions were optimized so that all the target compounds could get a higher sensitivity. Also, it could be applied to the analysis of the soil samples. The results showed good linearity with a correlation coefficient above 0.990 in the range of 2.0 μg/L to 50 μg/L. The determination limits of the contaminants were from 0.01 μg/kg to 0.22 -g/kg. And the recovery rates of blank samples of diatomite were between 71.2% and 118%. Seven parallel samples were determined and the relative standard deviations （RSD） were between 1.9% and 7.3%. When determining the 6 practical soil samples in Xuzhou using this method, OPCs and PAHs were detected, the ∑OPCs residues ranged from 2.9 μg/kg to 5.0 μg/kg. The ∑PAHs residues ranged from 10.2 μg/kg to 20.3μg/kg.