This paper studies the method of determinating content of Non- starch polysaccharides( NSP) in different varieties of naked oats in Derivatization- Gas Chromatographic. Silylation derivatization method was confirmed and chlorotrimethylsilane?would be used as derivative reagent through the exploration on the derivative methods,reagents and conditions. Optimal derivatives as well as ideal chromatographic Mararate peak of both monosaccharide standard substance and NSP extract of naked oats would be obtained when deriving in 80 ℃ for 80 min. The linear correlation coefficient of the method is between 0. 99584- 0. 99909. The method would be applied to the Mararation and determination of relevant monosaccharide composed of soluble and non soluble non- starch polysaccharide in naked oats and provides theoretical basis for the further analysis of other monosaccharide composition of NSP.