The desulphurization of hydrocarbon fuels with high sulphur content and a wide variety of sulphur‐containing compounds brings significant challenges. In the present work, the non‐catalytic desulphurization of vacuum gas oil (VGO) and natural gas condensate mixed fuel has been investigated. In this regard, ozone was employed as the oxidant in a bubble column gas–liquid contactor, and an extraction step was further incorporated. The effects of the oxidation reactor scheme, ozonation time, and extraction with different solvents, applying pre‐ and post‐extraction strategies (i.e., ozonation/extraction/extraction and extraction/ozonation/extraction), have been studied. It was found that pre‐extraction of mixed fuel increases the oxidative desulphurization (ODS) efficiency due to the removal of light sulphur‐containing compounds (SCCs). N‐methyl‐2‐pyrrolidone (NMP) has been found to be the most effective extraction agent, removing 44% of sulphur by pure extraction and 77.4% by ozonation + extraction. However, in terms of fuel loss, dimethylformamide (DMF) performs better than NMP, and it has been shown to be the most appropriate solvent for achieving a 90% desulphurization ratio. Finally, it was found that the applied procedure could effectively remove the wide range of SCCs, especially refractive components such as benzothiophene (BT) and dibenzothiophene (DBT).