毛细管气相色谱法测定那格列奈中有机溶剂的残留量

Determination of residual organic solvents in Nateglinide by capillary gas chromatography

目的建立测定那格列奈中有机溶剂残留量的方法。方法采用DB-WAX(聚乙二醇)毛细管柱(30.0m×530μm×1.0μm),程序升温法测定那格列奈中甲醇、丙酮、乙酸乙酯及三氯甲烷的残留量。其中,三氯甲烷采用电子捕获检测器(ECD),其余有机溶剂采用氢火焰离子化检测器(FID)。结果 4种残留溶剂完全分离,线性关系和回收率良好,3批样品检测残留溶剂均未超标。结论所建立的方法准确、灵敏,可用于那格列奈原料药中残留有机溶剂的测定。

OBJECTIVE To establish a capillary gas chromatography method was developed to determine residual organic solvents in Nateglinide.METHODS A temperature programmed GC determination was performed on DB-WAX capillary column（30.0m × 530μm × 1.0μm） with ECD for trichloromethane,while FID for other residual solvents.RESULTS Under experimental condition,four residual organic solvents were thoroughly separated.Every solvent had a good linear relationship and recovery.None of residual organic solvent was found to exceed quality limit in Nateglimide.CONCLUSION The method is accurate and sensitive for the determination of residual organic solvents in Nateglinide.