Abstract: In addition to the antitumor-active esters, 11-hydroxycephalotaxine and desmethylcephalotaxinone which were not resolved on packed column were successfully separated with SCOT glass capillary coated with OV-17 at 268℃. The crude alkaloid mixtures extracted from Cephalotaxus plants from four regions were analysed, and(GC)²-MS was used to identify four components in the crude alkaloid mixtures extracted from Cephalotaxus plant of region A, one of them seemed to be a newcompound of Cephalotaxine ester type. The quantitative glass Capillary gas chromatography of the mixtures of harringtonine and homoharringtonine showed that there was a great error in direct UV spectrometry.