Longhu Rendan pills (LRPs), a traditional Chinese over-the-counter medicine, have been used for the prevention and treatment of heatstroke and motion sickness. A sensitive, specific, and accurate headspace-solid-phase dynamic extraction method coupled to gas chromatography-tandem mass spectrometry (HS-SPDE-GC-MS/MS) was developed and validated for the investigation of the pharmacokinetic properties of L-menthol, borneol, isoborneol, and the metabolite camphor in rats after oral administration of LRPs. Target compounds were extracted using an SPDE needle device coated with a polydimethylsiloxane solid phase. Detection of components was achieved by GC-MS/MS in multiple reaction monitoring mode. This method was successfully applied in the evaluation of the pharmacokinetics of components and a metabolite of LRPs after a single intragastric administration of a 0.92 g kg À1 dose to rats. Pharmacokinetic parameters were calculated from the plasma concentrationtime data. C max values of L-menthol, borneol, isoborneol, and camphor in rat plasma were determined to be 876 AE 341, 268 AE 149, 158 AE 91, and 126 AE 56 ng mL À1 , respectively, and the AUC 0-t values were measured as 876 AE 259, 408 AE 121, 140 AE 50, and 401 AE 35 ng h mL À1 , respectively. These results provide useful information on the effective components of LRPs.