The present study investigated physicochemical properties and antioxidant activities in vivo and in vitro of purified compound polysaccharides (CPs-1) from Chinese herbal medicines, composed of lotus leaf, hawthorn, Fagopyrum tataricum, Lycium barbarum, Semen cassiae, and Poria cocos with the mass ratio of 2 : 4 : 2 : 1 : 1.5 : 1. The HPGPC profile and FT-IR spectra indicated that the average molecular weight of CPs-1 was 38.7 kDa and possessed the α- and β-D-pyranose, respectively. The methylation analysis and NMR spectrum demonstrated that CPs-1 had a →6)-β-D-Glcp-(1→6)-β-D-Glcp(1→ backbone. Furthermore, the antioxidant assays in vitro revealed that CPs-1 displayed high scavenging abilities for DPPH, hydroxyl, and reducing power, as well as ABTS and superoxide scavenging capacity. The antioxidant experiments in vivo revealed that CPs-1 could significantly enhance CAT, SOD, and GSH-Px activities and dramatically reduce MDA levels in liver and serum of high-fat mice. Therefore, CPs-1 could be potentially incorporated into pharmaceutical products or functional foods as a natural antioxidant.