An analytical procedure has been developed for the gas chromatographic determination of phenylpropanolamine hydrochloride (PPA. HCl) using acetylacetone (AA) as derivatizing reagent. Elution is carried out from the column HP-5 (30m X 0.32 mm i.d) with film thickness 0.25 µm at initial column temperature 70°C for 5 min, followed by heating rate 10°C/ min up to 120°C with total run time 20 min. Injection port and detector temperatures were maintained at 270°C and 300°C. Nitrogen flow rate was 2ml/ min and detection was by FID.  The split ratio was 10:1. The linear calibration was obtained with 50 to 750 µg/ ml PPA with detection limit of 15 µg/ ml. Under the condition ephedrine did not form, the derivatives with AA but separated from PPA derivatives. The linear calibration curve for ephedrine was obtained with 225-903 µg/ ml with detection limit of 103 µg/ ml.The method was used for the determination of PPA from Sinutab and Tavegyl -D tablets, and ephedrine from Ephedrine tablets.  The coefficient of variation for the analysis of pharmaceutical preparation was obtained within 0.78 % to 0.89 %.