Abstract:Objective: The method of determining polysaccharides and their monosaccharides composition by CZE was established to provide a reference for discussing the effective substance of Polygonatum and Odoratum. Method: The degradation conditions of Polygonatum and Odoratum polysaccharides were optimized by orthogonal tests. The degradative monosaccharides, which were derived with 1-phenyl-3-methyl-5-pyrazolone (PMP), were separated and determined by CZE, and the results were compared with those which were determined by phenol-sulfuric acid method. Result: The Polygonatum and Odoratum monosaccharides all included xylose, arabinose, glucose, rhamnose, mannose, galactose, glucuronic acid and galacturonic acid. However, the ratio was significant different. Conclusion : The analysis of Polygonatum and Odoratum polysaccharides and the composition of monosaccharide by CZE are accurate and reliable with satisfactory results. The similarities and differences of the effectiveness were evidenced by their monosaccharide composition in some degree, and the results suggested that their clinical application could not be confused.