毛细管气相色谱法测定盐酸度洛西汀中5种有机溶剂残留

目的：建立盐酸度洛西汀中5种有机溶剂残留（甲醇、丙酮、异丙醇、乙酸乙酯、二甲亚砜）的分离测定方法。方法：采用HP—1（60m×0．53μm，5μm）毛细血管柱，以氮气为载气，FID检测器，采用程序升温，柱温为40℃，保持3min，以10℃·min^-1的速度升至160℃，保持12min，进样口温度200℃，检测器温度250℃，分流直接进样，外标法计算残留溶剂的含量。结果：甲醇、丙酮、异丙醇、乙酸乙酯、二甲亚砜均具有良好的线性关系，精密度的RSD均≤3．0％，平均回收率在97．1％～99．5％之间。结论：本法简单、准确、灵敏度高，适用于盐酸度洛西汀中5种有机溶剂残留的同时测定。

Determination of 5 Residual Organic Solvents in Duloxetine Hydrochloride by CGC

Objective： To establish a capillary gas chromatography method for the determination of five residual organic solvents （ methanol, acetone,isopropanol, ethylacetate and dimethyl sulfoxide） in duloxetinehy drochloride. Method ： Residual organic solvents in duloxetine hydrochloride were determinated by directed injection on an HP-1 capillary column （60 m× 0. 53μm,5. 00 μm） with an FID detector. The carrier gas was nitrogen gas. The injector temperature was 200 ℃ and the detector temperature was 250 ℃. The column temperature program was initial temperature 40℃ （holding 3 min） with the increase rate of 10 ℃· min^-1 to 160 ℃ （holding 12 min）. The assay of residual solvents was calculated by external standard method. Result： The calibration curves of methanol, acetone, isopropanol, ethylacetateand and dimethyl sulfoxide all showed good linearity. The RSDs of precision were all less than 3.0%. The average recoveries were between 97. 1%-99. 5%. Conclusion： The method is simple, accurate and sensitive, and can be used for detection of five residual solvents in duloxetine hydrochloride.