An ultrasonic extraction method was evaluated for a GC/MS determination of polyaromatic hydrocarbons (PAHs) and n-alkanes in airborne particulate matter, compared with the Soxhlet extraction method. Three airborne particulate samples collected at an industrial area of Kitakyushu City, a heavy traffic area of Kawasaki City, and Urban Dust (Standard Reference Material 1649) were extracted for seven PAHs and eight n-alkanes by both the ultrasonic extraction method with cyclohexane-ethanol (3 : 1) and Soxhlet extraction method with benzene-ethanol (3 : 1). Vehicle Exhaust Particulate (NIES No. 8) was also extracted for the compounds by the two methods. The results of the target compounds by the ultrasonic extraction method well agreed with those by the Soxhlet extraction method, except for the vehicle exhaust particulate.