Porous carbonaceous adsorbent was prepared by carbonization of saccharose in silica gel pores followed by leeching out of the silica matrix. The product of pyrolysis was then deactivated by hydrogenation. The resulting adsorbent shows intermediate sorption properties between those of the highly polar pyrolytic glassy carbon and the hydrophobic graphitized carbon. The microparticulate mesoporous carbon was examined for its use in capillary HPLC separations. The separation of selected stereoisomers in a 320 microm I.D. capillary column packed with the porous carbon particles is described and discussed. Additionally, the porous carbon filled with dextran gel was tested as a material for direct HPLC analysis of drugs in human serum.