Field desorption mass spectroscopy has identified five phencyclopeptines in the crude alkaloidal extracts of Ceanothus sanguineus. A new paired-ion performance in the expansion of these alkaloids is discussed. Amino acid analysis, electron impact mass spectroscopy, and 1H nmr spectroscopy have established the structures of six phencyclopeptines including two isomers. The structure of 2 has not been previously reported.