Abstract: The mixture (2 mL) of 0.20 mol·L^-1 HCl solution and ethanol (1+1) was evenly added onto the infiltrated Cambridge filter to balance for 2 h. A pretreated filter was placed on the front end of the cigarette holder, a standard filter was placed on the back of the cigarette holder. After cigarette suction was carried out by a straight-line smoking machine according GB/T 19609, the two filters were placed into 50 mL of 0.01 mol·L^-1 HCl solution and extracted by oscillation at 150 r·min^-1 for 40 min. The extract was filtered through a 0.45 μm aqueous filter and analyzed by liquid chromatography and ion chromatography. The detection limits (3s) of resorcinol, resorcinol, catechol, phenol, m-p-cresol, o-cresol and ammonia were in the range of 0.005-0.027 mg·L^-1. Values of recovery obtained by standard addition method ranged from 77.7% to 109%. The proposed method was used to determine the major phenolic compounds and ammonia in the mainstream of cigarette smoke, giving results were in consistency with those obtained by the standard tobacco industry method.