A determination method was developed for the quantification of polar organic compounds in atmospheric fine particles in Beijing City by GC-MS. The optimally reactive conditions of two derivative methods were set up. The related coefficients (R2) of standard curves were 0.995-1.000. The precise of the GC-MS was 1%-10%, and the quantified detection limits ranged from 0.1 to 4.0 ng x microL(-1) depending on the various standard compounds. The percent relative standard deviation of standards and atmospheric samples were 3%-20% and 3%-17%, respectively. The methods were applied for Beijing fine particle samples in summer, fall, and winter in 2002. Total 42 polar organic compounds were identified and quantified, including 30 n-aliphatic and n-alkenoic acid species, 5 aliphatic dicarboxylic acid species, 3 monosaccharide anhydrides, 3 steroids, and benzoic acid. The sources of these compounds were discussed.