Abstract: A method of gas chromatography was proposed for determination of monosaccharides in polysaccharide samples. The polysaccharide sample of 10.00 mg was hydrolyzed into monosaccharides at 100℃ for 5 h by 0.4 mL of 4 mol·L^-1 trifluoroacetic acid solution, and then the mixture was acetylated. The DB-5 column was used as the stationary phase, and the split flow ratio of 10:1 was used for the sample injection. Linear relationships between values of peak area and mass concentration of 6 monosaccharides were obtained in the range of 2.00-100.00 mg·L^-1, with detection limits (3S/N)in the range of 0.11-0.18 mg·L^-1. Test for recovery was made by standard addition method, giving results in the range of 88.0%-110%, and RSDs (n=6) of peak areas ranged from 1.3% to 2.3%.