AbstractRepresentative phenylalkylamines (six enantiomeric pairs) and amino acid methyl esters (five enantiomeric pairs) have been examined by gas chromatography‐mass spectrometry, in the form of theirN‐(R)‐α‐phenylbutyryl,N‐(S)‐α‐phenylpropionyl‐ andN‐(R)‐α‐chlorophenylacetyl derivatives. In most cases, satisfactory gas chromatographic resolution of the diastereomeric amides has been achieved on both SE‐30 and OV‐17 stationary phases. The phenylbutyramides and phenylpropionamides gave the more informative mass spectra (for characterization of the amines) but molecular ions we