The aim is to establish a method for determination of muscone in Xihuang capsules.A gas chromatog. method was developed by using an OV-17 column(30.0 m*0.32 mm*1μm) with inlet temperature at 200°C, FID detector, and temperature at 250°C.The initial temperature was kept at 150°C for 26 min, increased to 230°C at the rate of 20°C and maintained for 20 min.There was a linear relationship within the test range of 1.5∼299.2 mg·L-1(r=0.9998).The average recovery was 94.7% with RSD 1.3%.The method was proved to be accurate and sensitive, and could be used for drug quality control.