气相色谱法测定阿戈美拉汀原料药中乙酸和乙醚残留.PDFVIP

Drug Evaluation Research 第41 卷第11 期 2018 年11 月 ·2021 · 气相色谱法测定阿戈美拉汀原料药中乙酸和乙醚残留 1 2* 2* 2 邹孟瑶 ，赵丽娜 ，李银峰 ，靳朝东 1. 天津中医药大学，天津300193 2. 天津药物研究院，天津300193 摘 要：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×0.5 μm ），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1 μL ，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。 关键词：阿戈美拉汀；直接进样气相色谱；有机残留溶剂 中图分类号：R917 文献标志码：A 文章编号：1674-6376 （2018 ）11-2021-04 DOI ：10.7501/j.issn.1674-6376.2018.11.016 Determination of residual organic solvents in Agomelatine bulks drug by gas chromatography 1 2 2 2 ZOU Mengyao , ZHAO Lina , LI Yinfeng , JIN Chaodong 1. Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China 2. Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China Abstract : 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 lin