顶空进样-毛细管气相色谱法测定格列美脲原料药中5种溶剂残留的含量

Determination Five Kinds of Residual Organic Solvent in Glimepiride by Headspace Capillary Gas Chromatography

目的：建立采用顶空进样—毛细管气相色谱法对第3代治疗糖尿病药物磺酰脲类降糖药格列美脲原料药中正己烷、丙酮、二氯甲烷、甲醇和甲苯5种有机溶剂的残留量测定方法,为格列美脲原料药中5种有机溶剂的残留量提供科学检测方法。方法：采用顶空进样程序升温法,平衡温度为110℃,FID检测器,DM-5毛细管色谱柱（30m×0.32mm,0.25μm）进行检测。结果：5种有机溶剂在各自浓度范围线性关系良好（r=0.9958~0.9991,n=5）,最低检测限为0.58~11.8μg·ml^-1;定量限范围为1.9~47.3μg·ml^-1;3个浓度的平均回收率为95.1%~103.5%,（RSD=1.0%~5.1%,n=6）。结论：该方法灵敏简单、科学严谨、可操作性强、结果可靠,可用于实际生产格列美脲原料药中5种溶剂残留的测定分析。

Objective：To develop the headspace capillary gas chromatography method for the determination of residual organic solvents consisted of methanol,acetone,dichloromethane,n-hexane and toluene in Glimepiride.Methods：The samples were injected by headspace sampler with program heating and FID detector.The determination was performed on DM-5GC capillary column（30m×0.32 mm,0.25μm）.Results：Linear response were obtained for methanol,acetone,dichloromethane,n-hexane and toluene in their respective concentration ranges（r=0.9958-0.9991,n=5）,and the limits of detection were 0.58~11.8μg·ml^-1,the limits of quantity were 1.9~47.3μg·m^-1.The average recoveries of three concentration levels were 95.1%~103.5%,with RSD=1.0%~5.1%（n=6）.Conclusion：The developed method is simple,sensitive,and accurate.It can be used for the detection of the residual solvents in glimepiride.