Abstract: A method for determining heterocyclic hydrocarbons in cigarette smoke through extraction with dichloromethane, clean-up with basic alumina SPE column, and qualitative analysis by GC/MS with heart-cutting two-dimensional columns was developed and compared with the results analyzed with one-dimensional GC/MS. The results showed that:1) heart-cutting effectively improved the separating ability of chromatography and had obvious advantage of one-dimensional GC in separation effects;2)the mass spectrum matching degrees of the target analytes increased significantly, it provides a good condition for accurate qualitative and quantitative analysis by mass spectrum.