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目的建立测定依帕司他原料药中残留有机溶剂甲醇、乙醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、甲苯的检测方法,为建立质量标准提供依据。方法采用DB-624毛细管柱(30 m×0.53 mm,3.0μm),氢火焰离子化检测器(FID),进样口温度210℃,检测器温度250℃,程序升温,流速3.0 m L·min~(-1),分流比10∶1,顶空平衡温度85℃,平衡时间30 min,按内标法(内标物叔戊醇)测定各残留溶剂的含量。结果药物中7种残留溶剂的精密度RSD均<5%,在各自的浓度范围内具有良好的线性关系,相关系数均>0.999,平均回收率为90.0%~100.0%。结论本方法专属性好,灵敏度高,操作简单,测定结果准确,适用于依帕司他原料药7种残留溶剂的同时测定。
OBJECTIVE To establish a method for the determination of residual organic solvents methanol, ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran and toluene in eptazepril raw materials and provide the basis for the establishment of quality standards. Methods DB-624 capillary column (30 m × 0.53 mm, 3.0 μm) and flame ionization detector (FID) were used. The inlet temperature was 210 ℃ and the detector temperature was 250 ℃. The temperature was programmed and the flow rate was 3.0 m L · min ~ (-1), split ratio 10: 1, headspace equilibrium temperature 85 ℃ and equilibrium time 30 min. The content of each residual solvent was determined by internal standard method (internal standard tert-amyl alcohol). Results The RSDs of the 7 residual solvents in the drug were all less than 5%. The correlation coefficients were all within 0.999 and the average recoveries ranged from 90.0% to 100.0%. Conclusion The method has good specificity, high sensitivity, simple operation and accurate determination. It is suitable for simultaneous determination of 7 residual solvents of epalrestat raw material.