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

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。

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

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.