In diethyl ether extracts from celeriac (Apium graveolens L. var.rapaceum) all four stereoisomers of (3a–7a)-cis-3-butylhexahydrophthalide were found to be present. The analyses were carried out by means of GC, enantioselective GC and GC-MS. The assignment of the relative configuration of the diastereomers3 and4 was accomplished by NOE difference spectroscopy.