GC法测定达沙替尼原料药残留溶剂

Determination of Residual Solvents in Dasatinib by GC

目的建立GC法检测达沙替尼原料药中残留溶剂的方法。方法色谱柱为HP-DB624毛细管柱(30 mm×0.53 mm,3.0μm),氢火焰离子化检测器(FID),载气为氮气;进样口温度:220℃;检测器温度:240℃;流速2 ml·min-1,采用程序升温:初温60℃,保持2 min,以20℃.min-1升温至80℃,保持2 min;以10℃·min-1升温至140℃,保持2 min;分流比为5∶1,直接进样,进样体积为1.0μl。以N,N-二甲基甲酰胺为溶剂,采用外标法测定。结果 4种溶剂均能达到较好的分离;峰面积与浓度呈良好的线性关系,精密度良好,回收率符合要求,3批样品检测残留溶剂均未超标。结论本测定方法简单,准确,可用于达沙替尼原料药中有机溶剂残留量的检测。

Objective To establish a method for determination of residual solvents in dasatinib by GC. Methods The residual solvents in dasatinib were separated by HP-DB624 capillary column （30 mm 0.53 mm, 3.0 μm） with the FID detector. The cartier gas was nitrogen. The injector temperature and the detector temperature were controlled at 220 C and 240 C ,respectively. The flow rate was 2 ml .min-1. The programmed column tem- perature was set as follows： maintaineded at 60 C for 2 min and then raised to 80 C at the rate of 20 C .rain-1 , the maintained for 2 min,before the temperature was finally raised to 140 C at the rate of 10 C .min-1 and main- tained for 2 min. The sample was dissolved in N, N-dimethylformamide. The split ratio was 5： 1. The injection vol- ume was 1 txl. Results The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision, accuracy and recovery. None of the residual organic solvents was found to exceed the quality limit. Conclusion The established method is accurate and reliable. It can be used for determination of residual solvents in dasatinib.