The bioassay-guided fractionation of the MeOH extract of Galla Rhois furnished two hepatoprotective compounds, an equilibrium mixture of 3-galloyl-gallic acid and 4-galloyl-gallic acid isomers (3), 1,2,3,4,6-penta-O-galloyl-beta-D-glucose (4), and two inactive phenolic compounds, gallic acid methyl ester (1) and gallic acid (2). Compounds 3 and 4 showed significant hepatoprotective effects with EC50 values of 70.39+/-5.4 and 29.51+/-0.7 microM, respectively, against tacrine-induced cytotoxicity, and 150.9+/-6.4 and 23.81+/-0.5 microM, respectively, against nitrofurantoin-induced cytotoxicity in Hep G2 cells.