Abstract: The unsaponifiable matters of the oil from Xanthoceras sorbifolia Bge are separated by TLC with silica gel G into four fractions: sterols, 4-methylsterols, triterpene alcohols and hydrocarbons. The acetates of sterols are separated by TLC with 18% silver nitrate impregnated silica gel G, using CH₂CL₂-petroleum (7:3 v/v) as developing reagents. The identification of major components is carried out by TLC, m.p.,optical rotation, GLC, IR spectrum and MS or GC-MS.It is found that Δ⁷-stigmastenol, α-spinasterol and Δ⁷-avenasterol are present in large amounts in the unsaponifiable fraction, α-spinasterol (purity 99.5%),Δ⁷-stigmastenol (purity 99.5%) Δ^5.22-stigmasterol (purity over 98%) and Δ⁷-avenasterol (purity 98%) in the sterol fraction are isolated and identified, while trace Δ⁵-sterols as campesterol, β-sitosterol and cholesterol are identified only.