Abstract: Seven major phenolic compounds, including hydroquinone, resorcinol, catechol, phenol, m+p-cresol and o-cresol, in mainstream cigarette smoke were determined by liquid chromatography with two-dimensional column(2D-LC). The conditions of heart-cutting and two dimensional chromatographic separation for resorcinol, and the stability of 2D-LC system were emphatically investigated. The deliveries of the phenolic compounds in mainstream smoke of twelve cigarette samples were tested with the developed method. The results showed that: 1)Resorcinol could be effectively separated from interfering substances by heart-cutting and 2D-LC. 2)The detection accuracy of the other phenolic compounds was not influenced. 3) The delivery of resorcinol in mainstream cigarette smoke of the test samples ranged from 0.72 to 2.15 μg/cig.