Chirality is a fundamental characteristic of all living organisms, and all essential biochemical processes exhibit enantioselectivity. Although enantiomers of one compound do not possess any physical differences, they show difference in physiological and chemical activity in biological systems. In general, one enantiomer of most of the racemic drugs shows significantly higher pharmacological activity than the other. In some cases one enantiomer can be totally inactive or in others, it can produce adverse side effects. Therefore, preparation and analysis of single enantiomer becomes important. This book deals with studies on direct and indirect enantioseparation of certain pharmaceutical compounds which are marketed as their racemic mixtures. These chiral compounds/ drugs are (RS)-Bupropion (Bup), (RS)-Baclofen (Bac), (RS)-Mexiletine (Mex) and (RS)-Fluoxetine (Flx). The enantiomeric separation carried out using different Chiral Derivatizing Reagents (CDRs), Chiral Stationary Phases (CSPs) and chiral selectors by means of Reversed Phase (RP)-HPLC, impregnated TLC or Chiral Ligand Exchange TLC has been discussed.