Abstract: AIM：To develop a GC-MS method for the study of pharmacokinetics of gemfibrozil in healthy human body. METHODS: A 25 m×0.2 mm ID HP-5 silica capillary column was used. The carrier gas was helium. The internal standard was ibuprofen. After acidification with 3 mol.L^-1 HCl solution, the plasma was extracted with n-hexane — dichloromethane (3∶1) and then reacted with bis-(trimethylsilyl) trifluoroacetamide (BSTFA). RESULTS: A good linearity was obtained from 0.4 to 60.0 μg.mL^-1 of gemfibrozil in human plasma (γ=0.9992). The detection limit of gemfibrozil in plasma was 0.1 μg.mL^-1. The average recovery was 96.5%. The pharmacokinetics of gemfibrozil was determined by this GC-MS method following a single oral dose of 600 mg gemfibrozil capsule given to each of 10 volunteers. The results showed that the plasma concentration-time courses conformed to one compartment model. CONCLUSION: The established GC-MS method was found to be a good method for determination of gemfibrozil in human plasma. The method was precise and sensitive.