毛细管气相色谱法测定新药ZLR-8原料中9种残留溶剂量  

Determination of Residual Organic Solvents in ZLR-8 by Gas Chromatography

作　　者：杨静[1] 刘文英[1] 张奕华[1] 黄海燕 李强 

机构地区：[1]中国药科大学,南京210009 [2]南京长澳医药科技有限公司,南京210007

出　　处：《江苏药学与临床研究》2005年第5期25-28,共4页Jiangsu Pharmacertical and Clinical Research

基　　金：国家自然科学基金资助项目(No.30271491)

摘　　要：目的采用气相色谱法首次同时测定ZLR-8[2-(2,6-二氯苯基氨基)苯乙酸-4-(4-苯基-1,2,5-NB023二唑-2-氧化物-3-)甲氧基苯甲脂]原料药中乙醚、石油醚(60 ℃～90 ℃)、正己烷、丙酮、乙酸乙酯、乙醇、二氯甲烷、乙腈及吡啶9种有机溶剂的残留含量.方法采用毛细管气相色谱法,以串联的石英毛细管柱EC-1000(酸改性聚乙二醇20 M,30 m×0.536 mm×3.00 μm)和AC-5(5%-二苯基-95%-聚二甲基硅氧烷,30 m×0.53 mm×1.0 μm)为色谱柱,程序升温,以二甲基甲酰胺为溶剂,甲醇为内标,FID检测器,气化室温度为200 ℃,进样口温度为250 ℃.结果 9种有机溶剂基本实现基线分离且线性关系良好(r均在0.9996以上),3批样品中9种有机溶剂的残留含量均符合要求.结论该方法灵敏、准确.AIM A gas chromatographic method was established to determine the contents of diethyl ether, petroleum ether, nhexane, acetone, ethyl acetate, ethanol, diehloromethane, acetonitrile and pyridine, the residual organic volatile solvents in ZLR-8 raw meterial. METHODS After dissolved in dimethylformamide,0.5 μl sample solution was injected on to a coupled EC-1000 and AC-5 capillary column with column temperature programmably increased and detected by FID detector. RESULTS The nine organic volatile solvents and the internal standard methanol were separated thoroughly. The linefity and range for nine organic solvents were satisfied. Three batches of samples were analyzed. CONCLUSION The method was proved to be accurate, sensitive and reliable. It is quite suitable to be used in the analysis of the organic volatile solvents in bulk pharmaceuticals.

关 键 词：气相色谱法 ZLR-8 有机溶剂残留量 

分 类 号：R927.1[医药卫生—药学]