Cholesterol is one of the more important compounds causing arteriosclerosis and other illnesses of the circulatory system. In this work we have developed a procedure for separating a mixture of sterols from commercial consumable fats and, as the next step, identifying the main components of the sterol mixture. The method of separation included conventional and over-pressure thin-layer chromatography and solid-phase extraction (SPE); capillary gas chromatography with mass spectrometric detection was the main method of identification. Sterols and sterol esters were separated from the fats by solid-phase extraction on Bakerbond aminopropyl or silica gel columns. Preli-minary identification of the isolated sterols was achieved by TLC in a DS-sandwich type chamber. Full identification of the isolated sterols was performed by GC-MS and quantitative estimation of the cholesterol content by capillary GC with flame ionization detection. The amount of sterols was found to be in the range 4.01-11.46 mg g-1 fat; the amount of cholesterol was 0-5.14 mg g-1 fat.