A mixture of sodium deoxycholate and beta-cyclodextrin has been used to resolve the enantiomers of the 1-cyano-2-substituted-benz[L]isoindole and dansyl derivatives of a variety of amino acids. The enantiomers of CBI-histidine and glutamic acid were resolved with this system unlike the case of gamma-cyclodextrin in combination with SDS reported in the literature. Dansyl derivatives have been generated in situ to provide information about the migration behavior of dansylic acid, a major by-product in the dansylation.