气相色谱法测定甲磺酸达比加群酯原料药中正己醇的残留量

Determination of Residuals of Hexanol in the Raw Material of Dabigatran Etexilate Mesylate by GC

目的：建立测定甲磺酸达比加群酯原料药中正己醇残留量的方法。方法：采用气相色谱法。以6%氰丙基苯基-94%二甲基聚硅氧烷（DB-624）为固定液的毛细管柱为色谱柱,氮气为载气,采用程序升温,进样口温度为180℃,检测器（氢焰离子化检测器）温度为250℃,氮气流速为8 ml/min,分流比为10∶1,进样量为1μl。结果：正己醇与溶剂峰及杂质峰能有效分离;其质量浓度在1~1 000μg/ml范围内与峰面积呈良好的线性关系（r=0.999 9）;方法检测灵敏度较高;精密度、重复性试验的RSD≤1.31%;平均加样回收率为102.40%,RSD=0.42%（n=9）。结论：该方法专属性强,操作简便快速,结果准确,能有效地排除主成分降解产生的正己醇干扰,可用于甲磺酸达比加群酯原料药中正己醇的残留量测定。

OBJECTIVE：To establish a method for the determination of hexanol residuals in the raw material of dabigatranet exilate mesylate. METHODS：GC was performed on the column of 6% cyanopropylphenyl-94% dimethyl polysiloxane（DB-624）as the stationary phase capillary column,the carrier gas was nitrogen,using the temperature program. The temperature of inlet was180 ℃,detector was hydrogen flame ionization detector with the temperature of 250 ℃ at the flow rate of 8 ml/min,split ratio was 10 ∶ 1 and the volume was 1 μ l. RESULTS：Hexanol can be effectively separated with solvent peak and impurity peak;there was a good linear relationship between the quality concentration and the peak area in the range of 1-1 000 μg/ml（r=0.999 9）. The method had high sensitivity. RSD of precision and repeatability test was no more than 1.31% and the average recovery was102.40%（RSD=0.42%,n=9）. CONCLUSIONS：The method is specific,simple,rapid,accurate,and can effectively exclud hexanol interference generated by degradation. It can be used for the determination of residuals of hexanol in raw materid of dabigatran etexilatem esylate.