[Analysis of solvent residues in raw material drug of glimepiride by head-space sampling-capillary gas chromatography].

An analytical method for the solvent residues in the raw material drug of glimepiride has been established by head-space sampling capillary gas chromatography. General evaluation was made for the distribution of organic residual solvents in glimepiride samples from 8 different domestic manufacturers. Based on the evaluation-test results and the information provided by manufacturers, 14 target solvents were ascertained including acetone, ethyl acetate, methanol, isopropanol, ethanol, chloroform, toluene, 1,4-dioxane, pyridine, chlorobenzene, ether, dichloromethane, n-hexane and benzene. The target solvents were divided into two groups for baseline separation according to their column-retention specificity. Acetone, ethyl acetate, methanol, isopropanol, ethanol, chloroform, toluene, 1,4-dioxane, pyridine and chlorobenzene were separated on a Supelco-Wax capillary column with acetonitrile as internal standard, while ether, dichloromethane, n-hexane and benzene were determined on a Supelco OVI-G43 capillary column with butanone as internal standard. Linear responses were obtained for the 14 residual solvents in their respective concentration ranges (r = 0.99167-0.99997, n = 8), and the limits of detection were 0.2-13.5 microg/g. The inter-day reproducibilities, measured as relative standard deviations (RSDs), were 0.6%-9.2% (n = 3). The average recoveries of three concentration levels were 86.3%-104.1% with the RSD of 0.2%-5.3% (n = 16). The developed method is simple, sensitive, and accurate for the residual solvent analysis in glimepiride samples.