气相色谱法测定阿戈美拉汀原料药中乙酸和乙醚残留

Determination of residual organic solvents in Agomelatine bulks drug by gas chromatography

目的建立测定阿戈美拉汀原料药中残留的2种有机溶剂(乙酸、乙醚)的检测方法。方法采用直接进样气相色谱法,色谱柱为DB-FFAP毛细管柱(30 m×0.32 mm×0.5μm),载气为高纯度氮气;柱温40℃,维持2 min,以50℃/min升至120℃;再以20℃/min升至220℃,维持2 min;氢火焰离子化检测器(FID),进样口温度为250℃,检测器温度为250℃,载气流量为2 mL/min,进样量1μL,分流比为20∶1。结果在考察的浓度范围内线性关系良好(r=0.999 7~0.999 8),2种残留溶剂均完全分离,精密度试验RSD值以及被测组分的平均回收率均符合要求。结论该气相色谱法操作简单,准确度、灵敏度高,可用于检测阿戈美拉汀原料药中残留的有机溶剂。

Objective To establish a method for determination of the two residual organic solvents, including acetic acid, diethyl ether in Agomelatine bulks drug.Methods Direct injection gas chromatography was applied to this study. The column was DB-FFAP silica capillary column(30 m × 0.32 mm × 0.5 μm) and the carrier gas was high purity nitrogen. The column temperature was kept at40℃ for 2 min, then the temperature was raised to 120℃ at the rate of 50℃/min, then the temperature was raised to 220℃ at the rate of 20℃/min and sustained for 2 min. FID detector temperature and injection temperature were both 250℃. The N2 flow rate was2.0 mL/min. The injection volume was 1 μL. The split ratio was 20:1.Results Two kinds of solvents were completely separated and determined with a good linearity(r = 0.999 7—0.999 8). The RSD values of precision experiments and the average recovery was in line with the requirements. Conclusion The analytical method is simple, accurate and sensitive, which could be used for determination of residual organic solvents in Agomelatine bulks drug.