Thin-layer and gas-chromatographic methods are described for the detection of 4-methyl-2,5-dimethoxy-alpha-methylphenethylamine in the submicrogram range. Cliromatographic criteria of identity for this new hallucinogen and for the related amines, amphetamine, methamphetamine and mescaline, and the hallucinogens, dimethyltryptamine and bufotenine, are also reported.