格列奇特中残留溶媒甲醇、乙酸乙酯的测定  

The residual solvents detection of methanol and ethyl acetate of Giiclazide

作　　者：李朝庆[1] 林萍[1] 屈海涛[1] 

机构地区：[1]哈药集团制药总厂,150086

出　　处：《黑龙江医药》2004年第3期175-176,共2页Heilongjiang Medicine journal

摘　　要：目的:建立一种气相色谱法测定原料药格列奇特中甲醇和乙酸乙酯有机溶剂残留量的方法。方法:选正丙醇作内标物,以 N,N-二甲基甲酰胺为溶剂在极性弹性石英毛细柱上进行各组分分离,效果良好。(采用程序升温)柱温100℃保留3分钟,以25℃/min 的速率升160℃保留5分钟。进样口温度200℃,检测器温度250℃,分流比70:1。载气:高纯氮气,流速:2.0ml/min。结果:平均回收率甲醇105.1%乙酸乙酯101.5%。结论:该方法克服了进样量不准确的缺点,重现性好,精度高。We detected the methanol and ethyl acetate content of Gliclazide using gas chro- matography(GC)method.Method:We used propan-l-ol as internal standard substance.The inter- nal standard substance and the sample tested were dissolved in N,N-dimethylformamide.The Chromatographic condition are carried out as following:the flexibility quartzose capillary column, temperature of the column 100℃ maintaining 3 minutes and 25 C/min increased temperature rate to 160℃ Maintaining 5 minutes,the temperature of the injection port 200℃,the temperature of the detector 250℃,the diffluent ratio 70:1,the carrier gas nitrogent and the flow rate 2.0ml/ min.The result showed the average recovery rate of acetone is 105.1% and the precision is better 101.5%.

关 键 词：格列奇特 甲醇 乙酸乙酯 测定 有机溶剂 残留量 气相色谱法 降血糖药 

分 类 号：R927.1[医药卫生—药学] R977.15