Abstract: Methacrylic acid (MAA)-trimethylolpropane trimethacrylate (TRIM) copolymer beads imprinted with tert.-butoxy-carbonyl-L-phenylalanine (Boc-L-Phe) have been prepared by suspension polymerisation in a perfluorocarbon liquid. The suspension polymerisation procedure has been adapted to work with a number of different porogenic solvents, and with UV initiated or thermal initiated polymerisation. The resulting polymers have been evaluated as stationary phases for the chromatographic separation of Boc-D,L-Phe. Polymer beads of average diameter 8-25 mu m packed into 100X4.6 mm chromatography columns were used with a mobile phase of dichloromethane-acetic acid (99:1, v/v) at flow-rates up to 5 mi min(-1). A polymer prepared with 1,2- dichloroethane as porogenic solvent (average bead diameter 15.1 mu m) was capable of the baseline separation of 100 mu g Boc-D,L-Phe at a flow-rate of 0.5 mi min(-1). (C) 1997 Elsevier Science B.V