Two methods for the determination of the enantiomeric ratio of verapamil in plasma by high-performance liquid chromatography have been developed. On an alpha 1-acid glycoprotein chiral stationary phase (Chiral-AGP) verapamil was separated after the acetylation of the main metabolite norverapamil, which interferes with the resolution of verapamil. On an amylose tris-3,5-dimethylphenylcarbamate column (Chiralpak AD) verapamil and norverapamil were determined simultaneously without prior derivatization. Gallopamil was separated on both columns under similar conditions.