The components of rocket kerosene were determined by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GCD GC/TOFMS) under pre-defined analytical conditions. Qualitative analysis was performed by identification of the various groups of the compound on a structured chromatogram. Quantitative analysis was performed by estimating the areas of the respective characteristic peaks. It was found that the kerosene contained paraffins, monocyclic, bicyclic, and tricyclic alkanes, alkenes, and aromatic and oxygen-containing compounds. It was demonstrated that GCD GC/TOFMS has obvious advantages over traditional methods for determining the components of rocket kerosene.