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ABSTRACTA new p-fert-butyl-calix[8]arene-bonded silica gel stationary phase was synthesized through heterogeneous functionalisation of suspended porous silica. A characterization of its structure was carried out by using elemental analysis, FTIR and 13C solid state NMR spectroscopy. Chromatographic performance of the new packing material was investigated by employing polycyclic aromatic hydrocarbons (PAHs) as probes and using methanol-water as mobile phase. The investigations show that the new stationary phase behaves as a reversed phase stationary phase. The liquid chromatographic separation of PAHs solutes on the new bonded phase was compared with that on a p-tert-butyl-calix[4]arene-bonded silica stationary phase. The new p-tert-butyl-calix[8]arene-bonded phase exhibited higher retention and better separation selectivity, although the carbon content and coverage of the new packing material was lower than that of the p-tert-butyl-calix[4]arene bonded silica stationary phase. A possible retention mechanism for the new packing material was also proposed.