A bis-substituted conjugate of the dichlorotriazinyl dye C.I. Reactive Blue 4 (Procion Blue MX-R) with 1H,1H-pentadecafluorooctylamine was synthesised and characterised. This novel conjugate showed strong surface activity on aqueous-fluorocarbon interfaces and was used to prepare dyed liquid and solid perfluorocarbon supports for affinity chromatography. Rabbit muscle lactate dehydrogenase was purified up to 8.4-fold from a crude extract by chromatography on the surface active dye adsorbed on perfluorodecalin emulsion droplets and on a powdered microparticulate fluoropolymer. The performance of these novel affinity supports was shown to be comparable to adsorbents prepared by using the same triazine dye immobilised on agarose gels. Two further surface active dichlorotriazinyl dye conjugates were immobilised on liquid and solid perfluorocarbon supports and tested using protein purification protocols to illustrate the applicability of this novel technique. © 1989.