Stems and leaves of Palicourea alpina were dried and powdered (150 g). Extraction with 2% tartaric acid followed by the usual work up for basic material yielded 0.275 g of crude material. PLC on silica plates using CHCl-MeOH (1:1) afforded 12 mg of a chromatographically homogeneous solid which had identical physical properties (UV, IR, NMR) to calycanthine. High resolution MS showed that the base peak was the parent ion (m/e 346.2113; Calculated for C22H26N4, 346.2157) and the fragmentation pattern observed was very similar to that reported earlier for calycanthine. Calycanthine has previously been shown to be the principal poisonous constituent of Calycanthus glaucus Willd. and was also reported from other Calycanthaceae species and Bhesa archboldiana (Celastraceae), but this is the first report of its isolation from the Rubiaceae. It is noteworthy that specimens of Palicourea alpina growing at Hardwar Gap, only 2 km from the location of the plants used in this study, did not yield this alkaloid, but other indole types were shown to be present.