Capillary-Gas Chromatographic Determination of Phenylpropanolamine Using Acetylacetone as Derivatizing Reagent in Pharmaceutical Preparations

An analytical procedure has been developed for the gas chromatographic determination of phenylpropanolamine hydrochloride (PPA. HCI) 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 I20°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 pharmaceuticalpreparation was obtained within 0 78 % to 0.89 %