The chromatographic method for the separation of racemic aminoacetonitriles and diamines, the intermediates in the synthesis of N-1-alkyl-1-arylethylenediamines derivatives, possessing biological activity, was elaborated on. The results of pharmacological testing were acquired so far only for racemic mixtures, so that a method, which would allow the control of purity, is required. The DNBPG chiral stationary phase (R-3,5-Dinitrobenzoyl-phenylglycine) was used for the enantioseparation of derivatives of aminoacetonitriles and diamines. Using a polarimetric detector the optical rotation of the separated enantiomers was determined. The effect of various substituents on the retention and enantioselectivity was investigated. The potential possibility of using a DAD detector in characterisation of the separated enantiomers and checking their purity was also investigated.