目的 建立測(cè)定阿戈美拉汀原料藥中殘留的2種有機(jī)溶劑（乙酸、乙醚）的檢測(cè)方法。方法 采用直接進(jìn)樣氣相色譜法，色譜柱為DB-FFAP毛細(xì)管柱（30 m×0.32 mm×0.5 μm），載氣為高純度氮?dú)?；柱?0℃，維持2 min，以50℃/min升至120℃；再以20℃/min升至220℃，維持2 min；氫火焰離子化檢測(cè)器（FID），進(jìn)樣口溫度為250℃，檢測(cè)器溫度為250℃，載氣流量為2 mL/min，進(jìn)樣量1 μL，分流比為20∶1。結(jié)果 在考察的濃度范圍內(nèi)線性關(guān)系良好（r=0.999 7～0.999 8），2種殘留溶劑均完全分離，精密度試驗(yàn)RSD值以及被測(cè)組分的平均回收率均符合要求。結(jié)論 該氣相色譜法操作簡(jiǎn)單，準(zhǔn)確度、靈敏度高，可用于檢測(cè)阿戈美拉汀原料藥中殘留的有機(jī)溶劑。

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 at 40℃ 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 was 2.0 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.