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The analysis of alkylbenzothiophenes (alkyl-BT) and alkyl-dibenzothiophenes (alkyl-DBT) in light cycle oil (LCO) and straight run (SR) gas oils is described. A detailed identification and quantitative analysis of alkyl-BT and alkyl-DBT present in LCO gas oils was carried out using GC-SCD. For the SR gas oils, the simultaneous presence of thiophenic and nonthiophenic compounds does not allow for a selective analysis of thiophenic compounds by GC-SCD. A new method using gas chromatography coupled with high-resolution mass spectrometry (GC-HRMS) is proposed to selectively detect and quantify the alkyl-BT and alkyl-DBT in SR gas oils. The development of the method and comparison of results between GC-SCD and GC-HRMS are presented.