A new chromatographic stationary phase has been prepared by cross polymerization between allylsilica and perallyloxycucurbit[6]uril and characterized by elemental analysis and FT-IR spectroscopy. The double endcapping has been proven to improve the separation efficiency of the cucurbituril-based stationary phase material. The first end-capping was carried out when allylsilica was made. The second end-capping was done as the final step of the whole process, and the use of a mixture of hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) as an end-capping reagent was found better than the use of only HMDS or TMCS. Our stationary phase has shown generally good results in separation of nonpolar and polar analytes. This phase showed even better separation performance than the commercial C18 phase for the case where hostguest chemistry was properly incorporated in solute retention.