The health benefits of whole grain consumption have been attributed to their content of complex carbohydrates, vitamins, minerals, and other phytochemical constituents. Wild rice is a whole grain finding applications in gourmet foods due to its nutritional value and unique taste. However, little is known about its antioxidant properties and phytochemical components. The objectives of this study were to evaluate the antioxidant properties of wild rice. Eleven commercial wild rice samples (raw, mixed, and processed) were extracted with acetone and fractionated using a Sephadex LH-20 column. 2,2-Diphenyl-1-picrylhydrazyl radical (DPPH(*)) scavenging activity, oxygen radical absorbance capacity (ORAC), and total phenolic content were evaluated to determine the antioxidant properties of wild rice. The antioxidant activity of wild rice was found to be 30 times greater than that of the control white rice. Significant differences (p < 0.05) in antioxidant activities were found among raw, mixed, and processed samples. For raw samples, DPPH(*) radical scavenging activities and ORAC values ranged from 611 to 917 micromol of Trolox equivalent (TE)/100 g and from 4069 to 6064 micromol of TE/100 g, respectively. For mixed and processed wild rice, DPPH(*) radical scavenging activities were 373 and 441 micromol of TE/100 g, respectively. The corresponding ORAC values were 2284 and 2557 micromol of TE/100 g. Total phenolic content (TPC) of raw wild rice varied from 2472 to 4072 mg of ferulic acid equivalent (FAE)/kg, higher than that of the mixed sample (1460 mg of FAE/kg) and processed sample (2076 mg of FAE/kg). TPC was highly correlated with total antioxidant activity of wild rice (r = 0.92). Tandem mass spectrometric techniques revealed the antioxidants identified in wild rice to be flavonoid glycosides (diglucosyl apigenin, glucosyl-arabinosyl apigenin, and diarabinosyl apigenin) in factions 2 and 3 and flavan-3-ols (catechin, epicatechin, and oligomeric procyanidin) in fractions 4 and 5.