气相色谱法测定富马酸卢帕他定中三乙胺的含量

Determination of Residual Triethylamine in Rupatadine Fumarate by Gas Chromatography

建立了富马酸卢帕他定原料药中三乙胺残留量的测定方法。采用顶空气相色谱法。色谱柱为CP-Sil8 CB(30 m×0.32 mm×1.00μm);氢火焰离子化检测器(FID),载气为氮气,流速为1.5 mL·min^(-1);检测器温度为250℃;进样口温度为150℃;柱温采用程序升温,初始温度40℃,维持5 min,再以20℃·m in^(-1)的速率升温至220℃,维持4 min;顶空瓶平衡温度80℃,平衡时间30 min。FID检测器测定三乙胺的残留量。结果表明,三乙胺在0.91~45.47μg·mL^(-1)(r2=0.9996)范围时线性关系良好,平均回收率为100.9%,RSD为1.7%(n=9),建立的方法准确、可靠、灵敏高,适用于测定富马酸卢帕他定原料药中三乙胺残留检测。

To establish a method for determination of residual triethylamine in Rupatadine Fumarate by GC. It was quantitatively determined by headspace gas chromatography （GC） with CP-Si18 CB column （30 m×0.32 mm×1.00μm）and FID detector. The carrier gas was nitrogen and the flow rate was 1.5 mL·min-1. The temperature of the injection port was maintaining at 150℃ and the temperature of detector was 250℃. The oven introduced sequential increasing of temperature programing. The initial column temperature was 40℃, maintained 5 min, then raised the temperature to 220℃ at a rate of 20℃·min-1, and maintained 4 min,. The headspace oven was set at a temperature of 80℃ for 30 min. Results showed that there was a good linearity within the range of 0.91-45.47μg.ml-1 for triethylamine. The correlation coefficient was 0.9996. The average recovery rate was 100.9 %. The RSD of precision was 1.7 %（n=9）, This method is accurate, reliable and sensitive for the determination of the residual quantity of triethylamine in Rupatadine Fumarate, and this method provides an idea for the determination of residual triethylamine in fumaric acid, citric acid, hydrochloric acid and other drugs.