Abstract: A sensory-oriented analysis was carried out to investigate the smoky components in total particulate matter (TPM) of mainstream cigarette smoke. The TPM of mainstream cigarette smoke was separated by gel permeation chromatography (GPC), the aroma characteristics of each separated fraction were estimated, and the fractions with characteristic smoky aroma were located. A total of 26 smoky components were identified by qualitative GC/MS analysis combined with aroma evaluation of standard substances, and a quantitative GC/MS method was developed for analyzing the 26 smoky components in TPM of mainstream cigarette smoke. The release of the 26 smoky components in mainstream smoke from cigarettes of 9 brands and their mass fractions in TPMs were determined. The olfactory thresholds of the 26 smoky components in ethanol and triacetin were determined by three-alternative forced-choice (3-AFC) method, and their odor activity values (OAVs) in TPMs of cigarettes of 9 brands were calculated on the basis of their mass fractions, then their contributions to the smoky aroma of cigarette smoke were estimated. The results showed that:1) In the mainstream smoke of the tested cigarettes, the release of phenol, 4-methylphenol, 4-vinylguaiacol, 2-methylphenol, 2, 4-dimethylphenol and tyrosol was higher than the other smoky components. 2) The contributions of guaiacol, 4-methylphenol and 5-methylguaiacol to the smoky aroma of cigarette were the most significant based on their OAVs.