This paper describes a highly sensitive and selective method for the determination of hydroxylated polycyclic aromatic hydrocarbons (PAHs-OH) in airborne particulates. PAHs-OH were extracted from airborne particulates with ethanol by ultrasonication. The extractant was further cleaned up by solid phase extraction (SPE) with an aminopropylsilica cartridge, and subsequently analyzed by reversed-phase high-performance liquid chromatography with fluorescence detection. 2-Hydroxy-1-acetonaphthone was used as an internal standard. By the proposed method, 2-hydroxyfluorene and 1-hydroxypyrene were identified in airborne particulates and their concentrations were determined for the first time.