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<p>Multi-oxygenated volatile organic compounds are important markers of air pollution and precursors of ozone and secondary aerosols in both polluted and remote environments. Herein, their accurate determination was enhanced. The approach was based on an automated system for active sampling and on-fibre derivatization coupled with the gas chromatography–mass spectrometry (GC–MS) technique.</p> <p>The method capability was determined for different compound families, such as aldehydes, ketones, <span class="inline-formula"><i>α</i></span>-dicarbonyls, hydroxy-aldehydes, hydroxy-ketones, and carboxylic acids. A good accuracy (<span class="inline-formula">&lt;7</span> %) was demonstrated from the results compared to Fourier-transform infrared spectroscopy (FTIR). Limits of detection (LODs) of 6–100 <span class="inline-formula">pptV</span> were achieved with a time resolution lower than 20 <span class="inline-formula">min</span>. The developed method was successfully applied to the determination of multi-oxygenated compounds in air samples collected during an intercomparison campaign (EUROCHAMP-2020 project). Also, its capability and accuracy for atmospheric monitoring was demonstrated in an isoprene ozonolysis experiment. Both were carried out in the high-volume outdoor atmospheric simulation chambers (EUPHORE, 200 <span class="inline-formula">m³</span>).</p> <p>In summary, our developed technique offers near-real-time monitoring with direct sampling, which is an advantage in terms of handling and labour time for a proper quantification of trace levels of atmospheric multi-oxygenated compounds.</p>