Abstract: α-Naphthyl isocyanate (NI), first introduced as an achiral derivatization reagent, has been successfully used for the separation of several chiral drugs of amines and alcohols on Pirkle-type CSP (DNBPG) column. Among these drugs, mexiletine, ketamine, benflumelol and phenylpropanol were first separated on Pirkle's column. The results show that this procedure using NI as an achiral derivatization reagent not only is quite convenient and gives good resolution, but affords derivatives With few impurities and avoids the desolution of the isocyanates. We can expect that this new derivatization reagent will be widely used in the field of resolution of enantiomers.