The dynamic flow profiles and column efficiencies in conically shaped semi-preparative liquid chromatographic columns (inlet ID larger than outlet ID) with two different conical angles (78 and 158) were studied. The dynamic flow profiles were studied by an on-column visualization method. Conical columns were compared with cylindrical column of the same length and internal volume. The results showed that the flow profile of a sample band in the conical column of 78 (50 mm617 mm 11 mm ID) was parabolic in shape. The sample band migrated slower in the wall region than in the central region, as in the cylindrical column (50 mm614 mm ID). However, the sample band in the conical column of 158 (50 mm620 mm 7 mm ID) migrated slower in the central region than in the wall region, resulting in a reverse parabolic flow profile, in contrast to that in cylindrical column. This indicated that a flat flow profile might be realized in a conical column with a conical angle between 78 and 158. The conical column of 158 had the highest column efficiency among the three columns under the same conditions. Compared with the cylindrical column packed with identical packing material, the conical column of 158 had 22% -45% higher column efficiency and 11% -27% higher peak height.