Determination of total ecgonine, formed by hydrolysis of crude cocaine with acid, was carried out. The ecgonine formed was adsorbed on strongly acid ion exchange resin (Amberlite IR-120), eluted with ammoniacal ethanol, and the ecgonine obtained was submitted to non-aqueous titration with perchloric acid solution in glacial acetic acid. Determination of cocaine by non-aqueous titration was carried out by adsorption of cocaine from ethanolic solution of crude cocaine on weakly acid ion exchange resin (Amberlite IRC-50), thereby separating cocaine alone from ecgonine and benzoylecgonine, eluted by ammoniacal ethanol, and titrated by the same method.