A simple proton nuclear magnetic resonance (PMR) spectroscopic method was developed for the quantitative determination of pipobroman in commercial tablets. Deuterochloroform was used as the PMR solvent and hexamethylcyclotrisiloxane served as the internal standard. The mean ± SD recovery value of pipobroman from synthetic formulations was 99.3 ± 0.49% of the added amount (n=9), with a coefficient of variation of 0.5%, The mean content of pipobroman in a group of commercial individual tablets was 99.2% by the PMR method and 99.7% by the titrimetric method of USP XX (n=11)