The efficacy of the carbon disulfide reaction in separating the tertiary amines from the primary and secondary amines was reevaluated by monitoring the separation by GLC and TLC techniques. The need of more than one method for the identification of dimethylated indoleamines is emphasized. 0-Phthalaldehyde is shown to be the most sensitive reagent for the qualitative identification of bufotenin and 5-Me0 DMT on TLC.