An accurate, simple and precise PMR procedure has been developed for the quantitation of benzyl benzoate (I) and benzyl cinnamate (II) as pure drugs and in Peru and Tolu balsams. The average recovery of pure I and II in standard mixtures using ethyl benzoate (III) as the internal standard was 100.2± 0.38% w/w and 100.0± 0.34 34% w/w respectively. The results of the assay using standard synthetic mixtures containing both I and II proved to be reproducible and gave a mean of 100.0 ± 0.54 w/w for I and 100.0 ± 0.62 w/w for II. Applying the same method for the determination of I and II in balsams, an average vlaue of 44.7% w/w was obtained for I and 4.4% w/w for II in Peru balsam. The corresponding average values for Tolu balsam were 11.6 w/w and 14.3% w/w. Moreover the method provides means for the ratio determination of I and II and the identification of the balsams.