Reactive oxygen species (ROS), in the form of superoxide anion(O 2 − ), hydroxyl radical (·OH) and hydrogen peroxide (H 2 O 2 ), are generated in living organisms through many pathways (Chung et al., 2005). An imbalance between production of ROS and their elimination in the organisms cause oxidative stress (Monika et al., 2010). Oxidative stress has been implicated as a possible factor in the etiology of several human diseases, including cancer, cardiovascular disease, Alzheimer's disease and aging (Suganya et al., 2007). Antioxidants are the important defense factors against oxidative stress caused by ROS. However, the use of synthetic antioxidant components, such as butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT), has been limited because of their possible toxic and carcinogenic effects (Branen, 1975). Thus, there is a growing interest in fi nding natural herbal plants with low in toxicity and high in radical scavenging activity (Branen, 1975). In the course of screening for antioxidant from Korean natural plants by measuring the radical scavenging effect on 1,1-diphenyl-2-picrylhydrazyl (DPPH), a total extract of the Galium spurium L. (Rubiaceae) was found to show a potent antioxidant activity. G. spurium is annual or biannual plant. Phytochemical studies on the genus have shown it to be chemically diverse, yielding among others, triterpenoid saponins, iridoidAs part of an ongoing search for natural plants with antioxidant compounds by measuring the radical scavenging effect on 1,1-diphenyl-2-picrylhydrazyl (DPPH), a total extract of the twigs of Galium spurium L. (Rubiaceae) was found to show potent antioxidant activity. Subsequent activity-guided fractionation of the methanolic extract led to the isolation of nine compounds, asperulosidic acid methyl ester (1), asperuloside (2), caffeic acid ( (8), and quercetin (9). Their structures were elucidated by spectroscopic studies. Compounds 1, 3-8 were isolated for the fi rst time from this plant. Among them, compounds 3 and 9 showed the signifi cant radical scavenging effects on DPPH, and compounds 3 and 7 showed the potent ribofl avin originated superoxide quenching activities. et al., 2000). Some iridoids (Deliorman et al., 2001), anthraquinones (Koyama et al., 1993) and fl avonoids (Cai et al., 2009) were analyzed from G. spurium. Its aerial parts have been used for the treatment of the bones and sinews pain and hematuria. Crude extract of G. spurium was also used as a anticancer agent in folk medicine. It has been reported to have immunostimulant and anti-tumor activity (Yoon et al., 2005). However, information concerning the antioxidant activity of G. spurium is unavailable. This paper deals with the isolation and structural characterization of these compounds and their scavenging activity of the stable DPPH free radical and superoxide quenching activities.