论文部分内容阅读
目的:建立气相色谱法测定阿戈美拉汀原料中有机溶剂残留量的方法。方法:采用FID检测器,色谱柱为Agilent DB-WAX毛细柱(30m×0.32mm,0.25μm),进样口温度180℃;检测器温度240℃,载气为氮气,柱温采用程序升温:初始温度40℃,保持10min,然后以20℃·min~(-1)的速率升温至200℃,保持5min,顶空瓶平衡温度80℃,平衡时间为30min。流速:1.06ml·min~(-1),以N,N-二甲基甲酰胺为溶剂。结果:异丙醚、四氢呋喃、乙酸乙酯、甲醇、二氯甲烷、乙醇与甲苯均能得到良好的分离,各自检测浓度在所考察的范围內与峰面积具有良好的线性;平均回收率为97.7%~101.1%(n=9)。结论:本方法简便、准确,灵敏度高,适用于阿戈美拉汀原料药中有机溶剂残留量的检测。
Objective: To establish a method for the determination of residual organic solvents in agomelatine raw materials by gas chromatography. Methods: FID detector was used. The column was Agilent DB-WAX capillary column (30m × 0.32mm, 0.25μm). The inlet temperature was 180 ℃. The detector temperature was 240 ℃. The carrier gas was nitrogen. The initial temperature was kept at 40 ℃ for 10min, then the temperature was raised to 200 ℃ at 20 ℃ · min ~ (-1) for 5min. The equilibrium temperature of headspace bottle was 80 ℃ and the equilibrium time was 30min. Flow rate: 1.06 ml · min -1, using N, N-dimethylformamide as a solvent. Results: Isopropyl ether, tetrahydrofuran, ethyl acetate, methanol, methylene chloride, ethanol and toluene could be separated well, and the linearity of the tested concentrations in the investigated range and peak area was good. The average recovery was 97.7 % ~ 101.1% (n = 9). Conclusion: The method is simple, accurate and sensitive. It is suitable for the determination of residual organic solvents in agomelatine APIs.