A rapid analysis of the sterol fraction of oils by on-line reversed phase liquid chromatography−gas chromatography (LC−GC) is described. Methanol:water is used as eluent in the LC preseparation step, 2000 μL/min being the speed of sample transfer. A programmed temperature vaporizer is used as an interface for the LC−GC equipment, and the solvent elimination is performed simultaneously in both the evaporative and nonevaporative modes so that a 3000-μL LC fraction can be transferred into the GC. The proposed procedure only demands previous dilution of the oil sample with CH2Cl2 and allows the analysis of the sterol fraction in only 20 min, including the oil sample preparation and the LC−GC analysis itself. Keywords: Reversed phase LC−GC; on-line coupling; sterols; direct injection; edible oils