顶空气相色谱法测定甲磺酸普依司他中三乙胺的残留量

Determination of Triethylamine in Purinostat Mesylate by Headspace Gas Chromatography

目的:建立甲磺酸普依司他原料药中三乙胺残留量的测定方法。方法:采用顶空气相色谱法,FID检测器,以6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的Agilent DB-624毛细管柱(30 m×0.53 mm,3μm),载气为氮气,流速为4.0 ml/min,进样口温度为200℃,检测器温度为250℃,柱温采用程序升温,初始温度为40℃,保持5 min,然后以10℃/min升至120℃,保持10 min,顶空条件为80℃平衡30 min,以二甲基亚砜(DMSO)为溶剂配制对照品溶液及样品溶液,采用外标法定量。结果:三乙胺浓度在0.64~12.8μg/ml内有良好的线性关系(n=5),平均回收率为101.4%(n=9),RSD为1.9%(n=9)。结论:本方法准确、可靠、灵敏度,适用于甲磺酸普依司他中三乙胺的残留量检测。

Objective： To determine the triethylamine in Purinostat Mesylate by GC. Methods： The residual triethylamine was determined by HS-GC with Agilent-INNOWAX capillary column（30 m×0.53 mm, 3 μm）and FID detector. The carrier gas was nitrogen and the flow rate was 4.0 mL/min. The temperature of the injection port was maintaining at 200 ℃, and the detector was maintaining at 250 ℃. The oven introduced sequential increasing of temperature programing. The initial column temperature was 40 ℃, maintained it for 5 min, then raised the temperature to 120 ℃ at a rate of 10 ℃/min, and maintained it at 120 ℃ for 10 min. The headspace oven was set at a temperature of 80 ℃ for 30 min. The solvent was dimethyl sulfoxide（DMSO）. The triethylamine was quantified external standard. Results： The calibration shows a good linearity with the range of 0.64-12.8 μg/mL for triethylamine. The average recovery was 101.4 %（n=9）, the precision was 1.9 %（n=9）. Conclusion： This method is accurate,reliable and sensitive for the determination of the residual quantity of triethylamine in Purinostat Mesylate.