Abstract: Samples of the "Jiuquhongmei" black tea (abbrev as black tea) and of the cut tobacco were ground and made to pass through sieve having 0.177 mm meshes separately, for preparation of analytical samples. 0.2 mg of the black tea sample or the tobacco sample was pyrolyzed at 200℃ under non-combustible condition, to liberate volatile components from the sample and to be carried over by He gas into the GC-MS instrumental system. After GC separation and MS determination, composition of the volatile components liberated from the 2 samples were obtained separately. Main components liberated from the cut tobacco sample were glycerol (59.34%, added artificially as smoking agent) and nicotine (20.34%), 3-butyne-1-alcohol (4.32%), 5-hydroxymethyl-furfural (3.23%), 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-ketone (2.12%) and etc. The main volatile components liberated from the black tea sample were caffeine (86.23%) and 16 characteristic components with low contents. A test was made by mixing the black tea with the cut tobacco at the mass percentage of black tea of 5%, 10% and 30%, and the variation of amounts of the liberated compounds from these black tea mixed tobacco was determined under the same pyrolytic condition, and sensory evaluation was also made. It was shown that amounts of caffeine liberated from the 3 black tea mixed tobacco samples was increased of 0.71%, 1.96% and 7.23% as the black tea contents increased from 5%, 10% to 30%, and the results of sensory evaluation were summarized as follows:Cigarettes made from black tea mixed cut tobacco were characterized by its merit of enhancing elegance of the cigarette smoke, strengthening the fruit, sweet and flower flavor of the cigarette, improving quantity and richness of its aroma, and also the fineness and softness of smoke, the after taste of sweetness. And it was found that in the case of addition of 10% of black tea, satisfactory taste with good after taste was already felt by smokers of the cigarettes, and overall promotion of sensory quality of comfort and coordination in smoking with appropriate aroma was attained.