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目的建立盐酸伊达比星原料药中残留溶剂的检查方法。方法采用毛细管色谱柱顶空进样气相色谱程序升温法测定。色谱柱为DB-624石英毛细管柱(30.0m×0.530mm,3.00μm);进样口温度:200℃;氢火焰离子化检测器(FID)温度:250℃;柱温:程序升温,初始温度50℃,保持6min,再以10℃·min-1的升温速率升至165℃,维持2.5min;载气:氮气;流速:4.0mL·min-1。顶空进样,平衡温度:105℃,平衡时间:20min,进样体积:1.0mL。以二甲基甲酰胺(DMF)为溶解介质。结果各被测溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系,方法的精密度良好,各溶剂的回收率较为理想。结论该法适用于盐酸伊达比星原料药的残留溶剂测定。
Objective To establish a method for the determination of residual solvents in idarubicin hydrochloride drug substance. Methods The capillary column headspace GC was used to determine the temperature. The column was DB-624 quartz capillary column (30.0m × 0.530mm, 3.00μm). Inlet temperature was 200 ℃. The temperature of FID was 250 ℃. The column temperature was programmed temperature and the initial temperature 50 ℃, hold 6min, and then heating rate of 10 ℃ · min-1 to 165 ℃, maintaining 2.5min; carrier gas: nitrogen; flow rate: 4.0mL · min-1. Headspace injection, equilibrium temperature: 105 ℃, equilibration time: 20min, injection volume: 1.0mL. Dimethylformamide (DMF) as the dissolution medium. Results The tested solvents could all be separated well. The peak area and concentration of each solvent showed a good linear relationship. The precision of the method was good and the recovery rate of each solvent was ideal. Conclusion The method is suitable for the determination of residual solvent of idarubicin hydrochloride.