抗血栓药物阿哌沙班中6种残留溶剂测定

Determination of Six Residual Solvents in Antithrombotic Drug Apixaban

目的：建立气相色谱法并测定抗血栓药物阿哌沙班中的残留溶剂。方法：以二甲基亚砜为溶剂,采用Rtx-Wax（0.32 mm×30 m,2.5μm）极性毛细管柱程序升温,以氮气为载气,FID为检测器,进样口温度为225℃,检测器温度为260℃,对阿哌沙班中6种残留溶剂（三乙胺、甲醇、异丙醇、甲苯、N,N-二甲基甲酰胺、甲酰胺）进行测定。结果：各被测残留溶剂均能良好分离、各溶剂线性关系良好,精密度RSD均不超过1.50%,平均回收率为96.0%~100.0%之间。结论：本文建立的方法可用于阿哌沙班原料药中残留溶剂的测定。

Objective： To establish a gas chromatography method for the determination of residual solvents in antithrombotic drug Apixaban. Methods： Six residual solvents including triethylamine, methanol, isopropanol, methylbenzene, DMF and formamide were determined by GC with Rtx-Wax capillary column（0.32 mm×30 m×2.5 μm, 2.5 μm） and an FID detector with 260℃. Temperature of the injection port was 225℃. Results： Each solvent could be completely separated in chromatography obtained from systemic suitability test, and the calibration curves of each solvent had a good linear relationship.The RSD of precision was not more than 1.50%.The average recovery was between 96.0% and 100.0%. Conclusion： GC method can be used to determine the residual solvents of Apixaban.