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A partially substituted β-cyclodextrin chiral stationary phase was prepared by the reaction of phenyl isocyanate. The enantiomers of a series of O,O-diethyl(p-methylbenzenesulfonamido)-aryl(or alkyl)-methylphos-. phonates were studied on the prepared phenyl carbamate derivative β-cyclodextrin bonded phase and a commercial ( S)-(.+ )-l-(l-naphthyl)ethylcarbamate derivative β-cyclodextrin bonded phase on normal phase chromato-graphic condition. Results show that the prepared phenyl carbamate derivative β-cyclodextrin bonded phase has better enantiomeric selectivity to the series of compounds. A chiral recognition mechanism was suggested for the separation of these novel organic phosphorus enantiomers.