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, CHl) using acetylacetone (AA) as derivatizing reagent. Elution is carred out from the column HP-5 (30m X 0.32mn i.d) with film thickness 0.25 mu m at initial column temperature 70 degrees C for 5 min, followed by heating rate 10 degrees C/min up to 120 degrees C with total run time 20 min. Injection pport and detector temperatures were maintained at 270 degrees C and 300 degrees C. Nitrogen flow rate was 2ml/min and detection was by FID. The split ration was 10:1. The linear calibration was obtained with 50 to 750 mu g/ml PPA with detection limit of 15 mu g ml. Under the condition ephedrine did not form, the derivities with AA but separated from PPA derivities. The linear calibration curve for ephedrine was obtained with 225-903 mu g/ml with detection limit of 103 mu g/ml. The method was used for the determination of PPA from Sinutab and Tavegl-D tablets, and ephedrine from Ephedrine tablets. The coeffient of variation for the analysis of pharmaceutical preparatation was obtained within .078% to .089%.