The ß-carboline compounds, harman (1-methyl-9H-pyrido[3,4-b]indole) and norharman (9H-pyrido[3,4-b]indole), occur in medicinal plants and in variety of food, alcoholic beverages, industrial waste and tobacco smoke. These compounds are synthesized by the reaction of indoleamine with some aldehydes under an oxidative condition. Concerning the tobacco smoke, norharman and harman are formed during the combustion by Pictet-Spengler condensation of tryptophan with formaldehyde or acetaldehyde. These ß-carbolines alkaloids exhibit a diverse range of pharmaceutical and biochemical activities. Here, we reported the development of a rapid and sensitive method to analyse harman and norharman in cigarette smoke condensates. In order to minimize sample handling and to decrease in analysis time, the method was developed for the direct injection of smoke condensate solution. For this, the analyses were carried out by liquid chromatography using fluorescence detection. Several chromatographic parameters were investigated, including the nature and the percentage of the organic solvent and acid modifier as well as column temperature. In-line sample preparation was also investigated and dimethylsulfoxyde appears to be the best solvent for a complete recovery. Moreover, this solvent is compatible with different in vitro test such as AMES test. The optimal conditions give a separation of harman and norharman in less than 10 minutes with a good resolution. In order to validate the method, precision was determined measuring the repeatability, accuracy and intermediate precision (between-day precision). Finally, the described method was applied to the quantitative analysis of harman and norharman in several cigarette smoke condensates.