Gas chromatographic, high performance liquid chromatographic and GC-ion trap detector mass spectrometric analyses of the hydroperoxides formed during thermal peroxidation of cholesteryl acetate, are reported and discussed. The hydroperoxides were separated from the thermal-oxidised mixture by solid-phase extraction, fractionated and individually collected by HPLC. Each hydroperoxide was then chemically reduced with NaBH4 to a hydroxy-derivative. The GC and MS characteristics of hydroxy- and TMS-derivatives were compared against available standards. Only 7β-hydroperoxide and 7α-hydroperoxide of cholesteryl acetate were found, as reported in the literature for cholesterol.
