盐酸文拉法辛残留溶剂检测方法的建立

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。

GC detection of residual solvents in venlafaxine hydrochloride

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 min.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 conditions,each solvent was completely separated in chromatogram 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 simple,accurate and reproducible.