Phenylpropanolamine (PPA) hydrochloride used as nasal decongestant agent was determined by second derivative spectrophotometry after derivatization with 2-hydroxynaphthaldehyde. The absorbance was measured between minimum-maximum of 386 nm-392 nm. The linear calibration range was obtained within 0.5~2.0 μg/mL. The method was applied for the determination of phenylpropanolamine from pharmaceutical preparations Tavegyl-D and Sinutab with coefficient of variation of 0.8~1.6%. Paracetamol present together with phenylpropanolamine could also be determined by spectrophotometry in aqueous phase after extraction of PPA in chloroform.