Abstract: A new method based on the off-line coupling of analytical SFE and GC has been developed for qualitative and quantitative analysis of major volatile components in Suhexiang Wan. a Chinese patent medicine. The factors affecting extraction efficiency were examined to seek the optimal operating parameters. Quantitative recovery (90%) was achieved with 20 ml CO₂ in ca I h using a self-designed analytical SFE system. Compared with the conventional methods, the SFE as an alternative technique for sample preparation will be most useful in the quality control of Chinese patent medicine.