A simple, rapid HPLC procedure was proposed for the separation and identification of Thioctic Acid and Thioctamide using Clofibric Acid as an internal standard. The procedure was performed using a reversed phase PC 8-10 column and a UV detector set at 250 nm. A mobile phase containing Acetonitrile and 1% Acetic Acid (40:60) was employed at a flow rate of 1 ml/min. Results showed that all of three chromatographic peaks were well separated. Capacity factors, selectivity factors and resolution factors of Thioctic Acid, Thioctamide and Clofibric Acid were reasonably acceptible.