Abstract Direct separation of the enantiomers of the two diastereomers, menthone and isomenthone, was performed using an octakis‐(3‐O‐butyryl‐2,6‐di‐O‐pentyl)‐α‐cyclodextrin phase. Enantiomerically pure (—)‐menthone and (+)‐isomenthone were detected in many oils of Mentha, Micromeria fruticosa (L.) Druce and Calamintha incána (Sm.) Heldr. High enantiomeric purities of (+)‐menthone and (—)‐isomenthone were detected in commercial and freshly distilled geranium oils.