An orthogonal array design (OAD) test, L9(3)4, including pressure, temperature, the mount of modifierandtheflowrateofCO2 wasperformedtogettheoptimalconditions.Theprocesswasthenscaled up by 30 times Supercritical fluid extraction (SFE) was used to extract cordycepin and adenosine from Cordyceps kyushuensis with a preparative SFE system under 40MPa, 40◦C, the mount of modifier (0.04mlmin−1) and a flow rate of CO2 (2.0lmin−1). The preparative SFE extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a selected two-phase solvent system composed of