A novel stationary phase is demonstrated for the separation of proteins. Capillary-channeled polymer (C-CP) fibers provide a stationary phase that is characterized by a high surface activity (yielding strong wicking action) and drastically reduced back pressures. Columns prepared by pulling approximately 1200 50- micro m diameter polypropylene C-CP fibers through stainless steel tubing with column dimensions of 4.6-mm i.d. and 306-mm length exhibit reversed-phase characteristics in the separation of the proteins. A gradient method [95:5 water-acetonitrile (ACN)/propanol (1:1) to 35:65 water-ACN/propanol] with trifluoroacetic acid added as an ion-pairing agent yields high-quality separations of superoxide dismutase, hemoglobin, hemocyanin, and myoglobin. It is believed that the C-CP fiber stationary phase holds a number of promising traits for applications in both analytical and prep-scale separations of diverse organic species, including a wide range of biomolecules.