Perbenzoylated gluco- and galactocerebrosides were separated and quantitated with a modification of existing HPLC methodology. A linear gradient of 0.9-18.4% dioxane in hexane was used to separate the derivatives on a pellicular silica column heated to 65 degrees C. The elevated temperature was the major modification that permitted the separation. This system was compared to a previously reported silica column/isopropanol in hexane system.