顶空气相色谱法测定头孢泊肟酯中三乙胺的残留量

目的建立头孢泊肟酯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,色谱柱为Elite-5-AMINE石英毛细管柱(30m×0.32mm,1.5μm),柱温采用程序升温,初始柱温为50℃,保持10min,再以20℃/min的速率升至200℃,保持5min,进样口温度为200℃,检测器温度为250℃,载气为氮气,流速为2.0mL/min,进样体积为1.0mL,分流比为5:1,平衡温度为80℃,平衡30min。结果在选定的色谱条件下,三乙胺的分离度在35以上,能够得到良好分离,0.531~10.617μg/mL范围内线性关系良好,r=0.9992;检测限为0.0265μg/mL,定量限为0.0796μg/mL;平均回收率为100.16%(RSD=3.38%,n=9)。结论该方法简便灵敏、结果准确、重复性好,适用于头孢泊肟酯中三乙胺残留量的检测。

Determination of residual triethylamine in cefpodoxime proxetil by headspace gas chromatography

Objective To establish a gas chromatography method for the determination of residual triethylaminein cefpodoxime proxetil. Methods The residual triethylamine was determined by the headspace gas chromatographyon an Elite-5-Amine (30m×0.32mm, 1.5μm) capillary column with an FID detector. The oven introduced sequentialincreasing of temperature programing. The initial temperature was kept at 50℃ for 10min, then raised the temperatureto 200℃ at the rate of 20℃ /min and lasted 5min. The temperature of injection port and the detector was 200℃ and250℃ , respectively. The carried gas was nitrogen at a flow rate of 2.0mL/min. The injection volume was 1.0mL andthe split ratio was 5:1. The headspace oven was set at a temperature of 80 ℃ for 30min. Results The resolutionof triethylamine was above 35, which can be well separated under the selected chromatographic conditions. Thelinear range of triethylamine was 0.531~10.617μg/mL, r=0.9992. The limit of detection was 0.0265μg/mL and thelimit of quantitation was 0.0796μg/mL. The average recovery was 100.16% (RSD=3.38%, n=9). Conclusion Themethod was simple, sensitive, accurate, and reproducible. It can be applied in the determination of triethylamine incefpodoxime