A simple and sensitive high-performance capillary electrophoresis (HPCE) method was designed for quantitative analysis of the component monosaccharides of an acidic polysaccharide extracted from pumpkin. In this method, the polysaccharide was hydrolyzed into component monosaccharides with 2.0 M trifluoroacetic acid at 100 degrees C for 6 h and then labeled with 1-phenyl-3-methyl-5-pyrazolone, and subsequently the labeled monosaccharide derivatives were separated by HPCE. As a result, glucose (21.7%) and glucuronic acid (18.9%) were identified to be the main component monosaccharides, followed by galactose (11.5%), arabinose (9.8%), xylose (4.4%), and rhamnose (2.8%). Furthermore, the pumpkin polysaccharide was also demonstrated to effectively inhibit the H2O2-caused decrease of cell viability, lactate dehydrogenase leakage, and malondialdehyde formation, and also reduced the H2O2-caused decline of superoxide dismutase activity and glutathione depletion in cultured mouse peritoneal macrophages, indicating that pumpkin polysaccharide possessed significant cytoprotective effect and antioxidative activity.