Abstract: GC/MS spectrometric analysis of 3 cigarette flavors was carried out with DB-5MS, DB-WAXETR capillary columns and coupling column systems composed of them. The results showed that: 1) the coupling column system with the total column length of 60m was superior than that of 80m in terms of isolation effect; 2) the polar-nonpolar coupling column system 60m in total length was better than a single polar or nonpolar column in the isolation of 2 of the flavors, and superior to a single nonpolar column but worse than a single polar column in isolating the other flavor. The polar coupling column system with an appropriate length was suitable for the isolation of some flavors; polar-nonpolar coupling column system was fit only for isolating those flavors which contained more polar components, less high boiling temperature components, and the middle-low boiling temperature components in which overlapped seriously in single column analysis. The disadvantages of coupling column systems includes: troublesome and time-consuming to be optimized; lower working temperature; parts of components isolated by precolumn likely to mix together again; and the negative effects of the dead volume in column connector on the separation of components.