Abstract: Capillary supercritical fluid chromatography (SFC)was developed for the determination of panaxadiol and panaxatriol in Radix notoginseng and Yunnan Baiyao. 0.1 g Radix notoginseng powder or 0.5 g Yunnan Baiyao was mixed with 10 ml 15% H₂SO₄ ethanol- water (1:1 )solution, adding 1 mg cholesterol as internal standard. The mixture was refluxed for 4 h, then adding 15 ml 15% NaOH solution, refluxed for 0. 5 h.The mixture was extracted 3 times with 10 ml portions of cyclohexane. The cyclohexane extracts were purified by partition column and concentrated by adsorption column and then analysed by SFC. The proposed method is sensitive, accurate, precise, simple and rapid;all the process can be done in 8 h.