Abstract: In order to accomplish the separation and determination of organic acids in tobacco flavors, a gas chromatography-mass spectrometry (GC-MS) method for the determination of oxalic acid, malonic acid, succinic acid, malic acid, palmitic acid, citric acid, stearic acid, oleic acid, linoleic acid and linolenic acid was developed by optimized the experimental conditions. The samples were derived with a 10% sulfuric acid-methanol (V/V) solution at room temperature for 24 hours, and then extracted with dichloromethane. The derived samples were analyzed by GC-MS under SIM mode and quantified by using adipic acid as internal standard. The results showed that: 1) Under the optimized conditions, the linear relationships of the target compounds in the respective linear ranges (R² > 0.998) were good, and the detection limits and quantification limits were in the ranges of 0.004-0.080 and 0.013-0.267 mg/kg respectively. The spiked recoveries of this method ranged from 83.06% to 110.29% with RSDs of 1.01%-6.50%. 2) Tobacco flavor samples of 26 kinds were analyzed using the developed method, it was found that the above ten organic acids were detected in most of the samples, and their contents in the flavors and those for casing were significantly different. 3) With the advantages of easy operation and higher sensitivity and precision, this method was suitable for the analysis of the ten organic acids in flavor samples.