This study was prepared to develop the sustained release dosage form of phenylpropanolamine hydrochloride (PPA) by complexation with cation exchange resin(CER). The PPA-CER complex was confirmed by differential scanning calorimetry(DSC) thermogram, indicating a relative shift of an endometric peak of PPA to higher temperature. The loading efficiency was increased as the amount of PPA was increased as well as the time of fractional exchange was advanced as the temperatures were increased. Loading efficiency, fractional exchange, reaction rate constant and activation energy were highly dependent on the temperature and drug : resin ratio. The optimal ratio of PPA and resin was estimated to be 10:10 for the sustained release.