In this review, some aspects of the separation of basic compounds by HPLC are discussed with especial reference to work carried out by the author. Procedures for column evaluation are explained, together with the effect of mobile phase modifier, pH, temperature, nature of buffer, and sample overloading on the chromatography of basic compounds. Some evaluations of new column types, such as embedded polar group phases, monoliths, and hybrid inorganic/organic phases are presented.