Abstract: Enrichment of organic sulfur compounds in gasoline was investigated with acid extracting agent (sulfuric acid + phosphoric acid + water) and solvent n-hexane. Sulfides and thiophene derivatives in gasoline are extracted into n-hexane; the concentration of sulfur compounds enriched in n-hexane can be higher than 12 times of the sulfur concentration in gasoline sample. Thus, sulfides and thiophene derivatives enriched in n-hexane can be analyzed easily by using a gas chromatography with flame photometric detector (GC-FPD) and a gas chromatographymass spectrometry (GC-MS) because of less interference of hydrocarbon. In this work, 52 sulfur compounds were detected with GC-FPD, of which 14 sulfur compounds with determinate structures were identified with GC-MS.