摘要
目的采用顶空进样气相色谱法测定西尼地平原料药中三乙胺和哌啶的残留量。方法采用程序升温法。色谱柱为SE-54毛细管柱（30.0 m×0.32 mm,1.0μm）,进样口温度200℃,氢火焰离子化检测器温度250℃,程序升温：初始温度50℃、保持5 min,以10℃·min^-1的速率升至70℃、维持2 min,再以40℃·min^-1的速率升至200℃。载气为氮气,流速1.0 mL·min^-1。顶空进样,顶空平衡温度70℃,顶空平衡时间30 min,顶空瓶中溶液体积3 mL,进样体积1.0 mL。以二甲亚砜为溶解介质,以乙酸乙酯为内标。结果三乙胺和哌啶的分离良好,各溶剂与内标峰面积的比值呈良好的线性关系,精密度良好,三乙胺和哌啶的RSD分别为1.5%、2.7%,回收率为99.9%～100.4%。结论所用方法适用于西尼地平原料药中三乙胺和哌啶残留溶剂的测定。
OBJECTIVE To establish a headspace GC method for determination of residual solvents （Triethylamine, Piperidine） in Cilnidipine. METHODS The residual solvents in Cilnidipine were determined by GC equipped with FID detector and linked with SE- 54 capillary column（ 30.0 m × 0.25 mm, 1.0 μm）. The injector temperature was 200 ℃ and the FID detector temperature was 250 ℃. The column temperature was rosen by program：The initial temperature was 50 ℃ ,maintained for 5 min, raised to 70 ℃ with a rate of 10 ℃ ·min^-1 ,maintained for 2 rain,and raise to 200 ℃ with a rate of 40℃·min^-1. The carries gas was nitrogen and the flow rate of carries gas was 1.0 mL·min^-1. The heated temperature of the headspaee oven was 70 ℃ , the heated time was lasted for 30 min, and the injection volume was 1.0 mL while the volume of headspace bottle solution was 3.0 mL. The dissolved medium used was dime- thyl sulfoxide and the internal standard was ethyl acetate. RESULTS Each solvent could be completely separated in ehromatogram obtained from systemic suitability test, and the calibration curve of each solvent had good linear relationship within a certain range. The method is accurate and reliable. The RSD of triethylamine and piperidine was 1.5% and 2.7% ,the recovery was between 99.9% - 100.4%. CONCLUSION The method could be applied in determination of the residual solvents in Cilnidipine.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2014年第5期596-598,共3页
West China Journal of Pharmaceutical Sciences
