Two new quaternary cactus alkaloids were detected in polar extracts of Coryphantha greenwoodii by tic. These alkaloids were crystallized and spectrally identified as N,N, N-triraethyl-4-methoxyphenethylamine chloride (O-methylcandicine, 1) and (+)-N,N,N-trimethyl-P-methoxyphenethylamine chloride (coryphanthine, 2). Synthesis of both compounds confirmed the structural identifications. Secondary ion mass spectrometry (sims) was invaluable in determining the molecular weights of these nonvolatile compounds. © 1983, American Chemical Society. All rights reserved.