An offline two-dimensional RP/RPLC system was developed for the separation of components in Dracaena cochinchinensis (Lour.) S.C.Chen xylem containing a resin that is an important raw material in Chinese traditional medicine. In this separation method, a CN-column was used in the first dimension and a C18-column in the second dimension. Fractions collected from the CN-column were resolved into many additional components, which indicated that the two-dimensional RP/RPLC system based on the CN- and C18-columns is orthogonal. The method provides higher peak capacity and better resolution. It is suitable for the analysis of complex samples such as those found in traditional Chinese medicines.