Abstract: To achieve accurate quantification and odor activity identification of sulfides in mainstream cigarette smoke, sulfides with odor activities reported in the research of food, environment, and agriculture were retrieved, and their union with those listed in the Rodgman & Perfetti list resulted in a target list of 65 sulfides. A quantitative method was established for 63 sulfides in the target list using GC-MS-MS combined with GC-MS, while semi-quantitative method was developed for carbonyl sulfide and hydrogen sulfide. A laboratory reference cigarette (Virginia type) and 1R6F reference cigarette (blended type) were analyzed. Based on the detection results, standard solutions were prepared to simulate the single-puff release of the smoke, and then the gas chromatography-olfactometry (GC-O) technology was used to analyze the odor characteristics of the sulfides in mainstream smoke, addressing the technical challenge of identifying odor characteristics of trace components in the complex smoke matrix. The results showed that 1) Among the 65 measured components, the intra- and inter-day RSDs for 62 target compounds were all no greater than 10%, indicating good method precision. The recovery rates of 61 target compounds ranged from 71% to 130%, indicating high method accuracy. The detection limits and quantification limits for 63 target compounds were 0.03‒45.88 ng/cig and 0.11‒131.95 ng/cig, respectively, indicating high sensitivity of the method. 2) In the laboratory reference cigarette smoke, 50 sulfides were identified, and 48 sulfides were detected in 1R6F reference cigarette smoke. Among these, 20 sulfides were not reported in the smoke components of Rodgman & Perfetti list. 3) Based on GC-O analysis, 21 sulfides in mainstream cigarette smoke were identified to be odor active by using the odor intensity method and the flavor dilution (FD) method. Among which, nine compounds including methyl mercaptan, 3-mercapto-2-pentanone, 3-(methylthio)propionaldehyde, dimethyl trisulfide, 2-acetyl-2-thiazoline, 2-mercapto-3-pentanone, furfuryl mercaptan, 2-methyl-3-mercaptofuran and thiophene-2-methanethiol made major contributions to the odor of cigarette smoke.