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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(60 m×0.53μm,5μm)毛细管柱,以氮气为载气,FID检测器,采用程序升温,柱温为40℃,保持3 min,以10℃·min~(-1)的速度升至160℃,保持12 min,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。
Objective: To establish a method for the separation and determination of five organic solvent residues (methanol, acetone, isopropanol, ethyl acetate and dimethyl sulfoxide) in duloxetine hydrochloride. METHODS: HP-1 (60 m × 0.53 μm, 5 μm) capillary column was used as the carrier gas and FID detector. The temperature of the column was kept at 40 ℃ for 3 min, 1) was raised to 160 ° C for 12 min, the temperature of the inlet was 200 ° C and the temperature of the detector was 250 ° C. Direct injection was performed by split flow and the content of residual solvent was calculated by external standard method. RESULTS: Methanol, acetone, isopropanol, ethyl acetate and dimethylsulfoxide all had good linear relationship. The RSD of precision was ≤3.0% and the average recovery was between 97.1% and 99.5%. Conclusion: The method is simple, accurate and sensitive. It is suitable for the simultaneous determination of five organic solvents residues in duloxetine hydrochloride.