The direct enantioseparation of 2-phenylpropanol, 2-phenylpropanal and 2-phenylpropanal dimethyl acetal was achieved, using enantioselective gas chromatography and heptakis-[2,3-di-0-acetyl-6-0-tert.butyldimethylsilyl]-β-cyclodextrin (DIAC-β-CD) or octakis-[2,3-di-0-acetyl-6-0-tert.butyldimethylsilyl]-γ-cyclodex-trin (DIAC-γ-CD) as the chiral stationary phase. Their odour characteristics and threshold values were investigated by enantioselective gas chromatography/olfactometry. Starting from commercially available (R)-2-phenylpropionic acid, enantiopure (R)-configured reference compounds were synthesi