The Miconia genus is the most representative of the Melastomataceae family, and some species are commonly used in Brazilian folk medicine as anti-inflammatory agents. In this work we investigated the leaves from Miconia rubiginosa (Bonpl.) DC, using high-speed countercurrent chromatography, which yielded 11 substances (eight flavonoids, gallic acid, casuarictin, and schizandriside). Identification was achieved using nuclear magnetic resonance spectroscopy and high-performance liquid chromatography-circular dichroism-diode array detection analyses.