Comprehensive two-dimensional gas chromatography utilising a semi-rotating cryogenic modulator was applied to the analysis of urban aerosols. Samples were collected onto glass fibre filters using a high-volume sampler in Helsinki, Finland. Sample preparation included extraction into n-hexane-acetone mixture and clean-up on silver-impregnated silica column. Analyses were performed with GC x GC-FID and GC x GC-QMS equipment. Linearity of the method was good with R2 values greater than 0.994 for all analytes. Polycyclic aromatic hydrocarbons (PAHs) and oxygenated polycyclic aromatic hydrocarbons (oxy-PAHs) were identified and quantified in urban particulates. PAH and oxy-PAH concentrations ranged from 0.5 to 5.5 ng/m3.