In this study we monitored benzothiazole (BTHs), benzotriazole (BTRs) and benzenesulfonamide (BSAs) derivatives in airborne particulate matter from four sampling sites near the port of Tarragona (Spain) over a one-year period. To do so, we developed a method based on ultrasound-assisted solvent extraction (USAE) followed by gas chromatography-mass spectrometry (GC-MS). We also studied concentrations of NO and airborne particulate matter (PM and PM) for a year. Our results showed NO and PM concentrations below the maximum average values established by the Europen Directive 2008/50/EC in the zone under study. Moreover, NO values are directly proportional to changes in weather conditions and traffic emissions, while PM and PM concentrations do not follow a clear trend as these may be generated from multiple sources (loading and unloading activities and traffic emissions). Regarding BTHs, BTRs and BSAs concentrations in particulate matter, the compounds found at the highest concentrations were 1-H-benzothiazole, 2-methylbenzothiazole, 2-chlorobenzothiazole, 1-H-benzotriazole, 4-methyl-1-H-benzotriazole, 2-(methylthio)-benzothiazole, 5-methyl-1-H-benzotriazole and bromobenzenesulfonamide with average concentrations ranging from 0.19 to 1.54 ng m in PM and from 0.09 to 0.61 ng m in PM. The remaining compounds were below the method quantification limits (MQLs) or were undetected in the samples analysed. Health risk values associated with the inhalation of the studied compounds were between 1.80 × 10 and 1.27 × 10 in the worst-exposure scenario.