盐酸文拉法辛残留溶剂检测方法的建立  

GC detection of residual solvents in venlafaxine hydrochloride

作　　者：袁斌[1] 王以武[2] 

机构地区：[1]川北医学院药物研究所川北医学院药学院,四川南充637000 [2]重庆医科大学药学院,重庆400016

出　　处：《川北医学院学报》2013年第1期13-16,共4页Journal of North Sichuan Medical College

基　　金：四川省教育厅科研项目(11ZB159)

摘　　要：目的:建立采用气相色谱法测定盐酸文拉法辛原料药中的乙醚、四氢呋喃、乙酸乙酯、甲醇、异丙醇、甲苯6种有机溶剂的残留含量方法。方法:采用Inowax色谱柱(30 m×0.32 mm×0.25μm),FID检测器,汽化室温度:150℃,检测器温度:250℃,进样量:1.0μL;柱温:程序升温:起始柱温40℃,保持7.5 min后,以50℃/min的升温速率升至120℃,保持3.5min;载气:高纯度N2,流速1.5 mL/min。以N,N-二甲基甲酰胺为溶解介质,乙腈为内标,对乙醚、四氢呋喃、乙酸乙酯、甲醇、异丙醇、甲苯6种溶剂进行检测。结果:被测各溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系;方法的精密度良好;回收率较为理想。结论:该方法操作简便、结果准确、重现性好,可用于盐酸文拉法辛残留溶剂的检测。Objective：To establish a method for the determination of the venlafaxine hydrochloride residues of six kinds of solvents by gas chromatography. Methods：The column is Inowax （30 m × 0.32 mm× 0.25 μm）, FID is used as the detector. The injector temperature is 150 ℃ and the detector temperature is 250 ℃. The injection volume was 1.0 μL. The column temperature was raised by program：the initial temperature was 40 ℃ ,maintained for 7.5 min was raised to 120 ℃ with a rate of 50 ℃/min, maintained for 3.5 rain. The carries gas was highly purified nitrogen, and the flow rate of carried gas N2 was 1.5 mL/min. The dissolved medium used to prepare all of the test solutions was N,N-dimethylformamide, and the internal standard was acetonitrile. Results： Under the above con- ditions, each solvent was completely separated in ehromatogram obtained from a systemic suitability test. The calibration curves of each solvent had a good linear relationship within a certain range, and the recovery rates was acceptable. Conclusion：The method is sim- ple, accurate and reproducible.

关 键 词：气相色谱法 盐酸文拉法辛 残留溶剂 

分 类 号：R94[医药卫生—药剂学]