Solid-phase microextraction in combination with gas chromatography and mass-spectrometry (GC-MS) was used for determination of benzene, toluene, ethylbenzene and o-xylene (BTEX), polycyclic aromatic hydrocarbons (PAH), and for identification of volatile organic compounds (VOCs) in ambient air of the city of Astana, Kazakhstan. The screening of the samples showed the presence of mono- and polycyclic aromatic hydrocarbons, alkanes, alkenes, phenols, and benzaldehydes. The concentrations of naphthalene were 5-7 times higher than the permissible value, it was detected in all studied air samples. Average concentration of naphthalene was 18.4 μg/m3, acenaphthylene – 0.54 μg/m3, acenaphthene – 1.63 μg/m3, fluorene – 0.79 μg/m3, anthracene – 3.27 μg/m3, phenanthrene – 0.22 μg/m3, fluorantene – 0.74 μg/m3, pyrene – 0.73 μg/m3. Average concentrations of BTEX in the studied samples were 31.1, 84.9, 10.8 and 11.6 μg/m3, respectively. Based on the statistical analysis of the concentrations of BTEX and PAH, the main source of city air pollution with them was assumed to be vehicle emissions.