OBJECTIVE: To establish the method for simultaneous determination of 5 volatile constituents in Shexiang zhuifeng zhitong plaster. METHODS: Gas chromatography was adopted. The determination was performed on PEG-20M capillary column with flame ionization detector as detector,nitrogen (99.999%) as carrier gas, with column flow rate of 1.5 mL/min, purge flow of 3.0 mL/min, split ratio of 5 ∶ 1, injector temperature of 200 ℃, detector temperature of 250 ℃, temperature programming, sample size of 2 μL, tail blowing flow of 40 mL/min. RESULTS: The linear range of camphor, borneol, isoborneol, menthol and menthyl salicylate were 19.78-247.26 μg/mL(r=0.999 6), 15.88-198.52 μg/mL (r=0.999 9), 8.60-107.56 μg/mL(r=0.999 9), 20.11-251.32 μg/mL (r=0.999 8)and 12.09-151.11 μg/mL (r=0.999 3), respectively. The limits of quantitation were 329.68,264.69, 143.41, 335.09, 402.96 ng/mL; the limits of detection were 98.90, 79.41, 43.02, 100.53, 120.89 ng/mL, respectively. RSDs of precision, stability and reproducibility tests were all lower than 3%. The recoveries were 97.85%-101.52%(RSD=1.54%,n=6), 99.55%-103.75%(RSD=1.38%,n=6), 98.88%-104.23%(RSD=1.94%,n=6), 98.11%-102.64%(RSD=1.92%,n=6), 96.55%-99.61%(RSD=1.44%,n=6), respectively. RSDs of durability test were all lower than 3%. CONCLUSIONS: The method is simple, precise, stable,reproducible and durable, and can be used for simultaneous determination of 5 volatile constituents in Shexiang zhuifeng zhitong plaster.