A method is developed for detection of polycyclic aromatic hydrocarbons (PAHs) and Phthalic Acid Esters (PAEs) in soil samples. Ultrasonic Wave Extraction under airtight circumstances is adopted to extract the analytes in soil samples with n-hexane–acetone (V:V=1:1) as extraction solvent. This method has several advantages, including high extraction efficiency, short time, convenience and simplicity. It can be used to detect polycyclic aromatic hydrocarbons (PAHs) and Phthalic Acid Esters (PAEs) in soil.