The ethyl acetate soluble fraction of an acetone/water extract of the air-dried aerial parts from Myrothamnus flabellifolia Welw. (Myrothamnaceae) was fractionated by a combination of CC on Sephadex LH-20, MPLC on RP-18 material and LPLC on MCI-gel. This procedure has led to the isolation of 2,3-di-O-galloylarbutin, a new representative of the rare 2,3-diacylated glucopyranosides. The structure was elucidated with the help of 2D-NMR and ESI-MS experiments. Conformation of D-glucose was established by CZE (capillary zone electrophoresis).