Abstract: GC-MS was applied to the determination of 6 volatile phenols, i.e. phenol, o-cresol, p-cresol, m-cresol, hydroquinone, and resorcinol, in mainstream smoke of cigarettes. The total particulate matter in mainstream smoke of 5 cigarettes were trapped by Cambridge filter pad under standard smoking condition and extracted ultrasonically with methanol for 10 min. The extract was separated on DB-624 capillary column (30 m×0.25 mm, 1.4 μm). Full-scanning mode and selected ion monitoring mode were adopted in MS determination. Phenol-D5 was used as internal standard. Detection limits (3S/N) of the method found were in the range of 10-16 ng·cig-1 each cigarette and lower limits of determination (10S/N) of the method found were in the range of 28-40 ng·cig-1 each cigarette. Values of recovery found by standard addition method were in the range of 84.6%-99.1%, and values of RSD′s (n=6) were found in the range of 2.1%-6.4%.