<p>Volatile organic compounds (VOCs) are key contributors to urban air pollution, photochemical smog, and associated health risks. Skopje, one of Europe’s most polluted capitals, faces significant VOC emissions from traffic, industry, and domestic heating. This study presents a year-long monitoring of 82 VOCs at five urban sites in Skopje, assessing concentrations, seasonal variability, emission sources, and ozone formation potential (OFP). Aliphatic hydrocarbons dominated, followed by aromatics (notably BTEX (benzene, toluene, ethylbenzene and xylenes)), terpenes, and hydrocarbon derivatives. Winter showed higher VOC levels due to heating, traffic, and industrial activity, while summer levels declined due to photochemical degradation and atmospheric dispersion. BTEX analysis, diagnostic ratios of toluene/benzene (T/B), and correlation patterns indicated traffic as the primary source, with industrial and waste-related contributions at specific sites. Principal component analysis identified six source-related factors: mixed traffic, solvent/industrial emissions, biogenic sources, fuel evaporation, personal care products, and industrial/petroleum-related VOCs. Meteorological factors also influenced VOC dynamics: aromatics and aliphatics correlated negatively with temperature, UV radiation, and ozone, while PM_2.5 correlated positively with aromatics and terpenes, linking VOC emissions to fine particulate matter. OFP analysis revealed that highly reactive species – toluene, xylenes, C₆-C₃ substituted benzenes, and <i>n</i>-tetradecane – disproportionately drive ozone formation, despite lower abundance. This work provides the first comprehensive VOC dataset for Skopje, revealing source contributions, seasonal patterns, and compounds with the greatest OFP. Findings support targeted air quality management, emphasizing control of high-OFP VOCs and integrated strategies considering both emissions and atmospheric chemistry to reduce urban pollution and associated health risks.</p> Graphical abstract <p></p>