氢溴酸西酞普兰原料药中10种残留溶剂的检查方法研究

目的：建立测定氢溴酸西酞普兰原料药中10种残留溶剂（甲醇、乙醇、丙酮、异丙醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、苯、甲苯）的方法。方法：采用顶空毛细管气相色谱法。色谱柱为DB-624毛细管柱;程序升温;载气为氮气,流速为2.0mL·min-1;进样口温度为200℃;检测器为氢火焰离子化检测器,检测器温度为250℃;顶空进样,顶空瓶平衡温度为85℃,平衡时间为30min。以二甲基亚砜为溶剂,用外标法测定10种残留溶剂的量。结果：在本色谱条件下,10种残留溶剂均能得到良好分离,在各自的浓度范围内具有良好的线性关系,相关系数均在0.9996及以上,平均回收率为95.7%～105.3%,RSD为1.6%～3.2%。结论：本方法简便、准确、重现性好,可用于氢溴酸西酞普兰原料药中多种残留溶剂的同时测定。

Study on Determination Method of 10 Kinds of Residual Solvents in Citalopram Hydrobromide Raw Materials

OBJECTIVE：To establish the method for the determination of residual solvents in citalopram hydrobromide raw materials,such as methanol,ethanol,acetone,isopropanol,carrene,n-hexane,acetic ether,tetrahydrofuran,benzene and toluene.METHODS：Head-space gas chromatography was adopted.The determination was performed on DB-624 capillary column at the flow rate of 2.0 mL·min-1,with temperature programming,using nitrogen as carrier gas.The temperature of injector was 200 ℃.Flame ionization detector was used and the temperature of it was 250 ℃.The containers of head-space injector were in equilibrium at 85 ℃ for 30 min.The dimethyl sulfoxide was solvent and external standard method was used for the determination of 10 residual solvents.RESULTS：Under the above condition,10 solvents were well-separated.There was good linear relationship in the concentration range,and correlation coefficients were no less than 0.999 6.The average recoveries were 95.7% ～105.3% with RSD ranged from 1.6% to 3.2%.CONCLUSION：The established method is simple,accurate and reproducible,and it can be used for the determination of residual solvents in citalopram hydrobromide raw materials.