Gas chromatog. for residual solvents detection in glibenclamide was established.The separation was carried out on an Agilent DB-624 column (30 m×0.32mm) and the sample was detected by flame-ionization detection (FID).The linear ranges for methanol, acetone and toluene were 75-600 μg·mL-1, 125-1000 μg·mL-1 and 22.2-178μg·mL-1, and the average recoveries were 97.7%, 98.0% and 98.9% with RSDs 2.1%, 1.0% and 1.2%, resp.The method is specific, simple and accurate, and is available for the residual solvent limit determination in glibenclamide.