OBJECTIVE：To establish a fully enclosed and free treatment quantitative analysis method for the contents determination of camphor and menthol in Prickly heat powder. METHODS： GC chromatography was conducted with internal standard of N-butanol and headspace solvent of 1-ethyl-3-methylimidazolium tetrafluoroborate. The column was PEG-20M capillary column， detector was hydrogen flame ionization detector， equilibrium temperature was 140 ℃， equilibrium time was 30 min， the column temperature was 160 ℃， the inlet temperature was 170 ℃， the detector temperature was 200 ℃， carrier gas was nitrogen， flow rate was 41 ml/min， split ratio was 18 ∶ 1， and the headspace volume was 1 ml. RESULTS： The linear range was 5.15×10－3-515 μg/ml（r＝0.998 4） both for camphor and 5.40×10－3-540 μg/ml（r＝0.998 2） for menthol； RSDs of precision， stability and reproducibility tests were lower than 2％； recoveries were 99.0％-101.3％（RSD＝0.9％，n＝9） and 98.3％-101.9％（RSD＝1.2％，n＝9）， respectively. CONCLUSIONS： This method is simple， accurate， sensitive and reproducible， and can be used for the contents determination of camphor and menthol in Prickly heat powder， which provides an accurate and reliable analysis method for the quantitative analysis of semi-volatile components in solid pharmaceutical preparations.