Abstract: According to national standards of soil environmental quality standard (GB 15618-1995) and the determination of polycyclic aromatic hydrocarbons in soil and sediments by gas chromatography-mass spectrometry (HJ 805-2016),8 kinds of organochlorine pesticides (OPCs) and 16 of polycyclic aromatic hydrocarbons (PAHs) in soil were selected as the research objects. Two pretreatment techniques,solvent selection and two different matrix dispersants for organic matter detection in soil samples were analyzed and compared. The gas chromatograph-three weight four lever mass spectrometry detection method was as follows: based on fast solvent extraction,60 mesh diatomite was used as matrix dispersant,and the rate of acetone and n-hexane (1∶ 1) was used as extractive solution. After 4 times of extraction when the volume ratio of 99%,it was purified by floret silica column. The recovery rate was 49. 92% ～ 128. 28%,and the detection limit was 0. 00109 ～ 0. 00651 mg/kg,which met the requirements of practical analysis. This method has the characteristics of simple and rapid,and shortens the pretreatment and analysis time. It has reference for the detection of polycyclic aromatic hydrocarbons and organochlorine pesticides in soil.