氢溴酸西酞普兰原料药中10种残留溶剂的检查方法研究  

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

作　　者：洪志玲[1] 胡猛慎[1] 

机构地区：[1]厦门市药品检验所,福建厦门361012

出　　处：《中国药房》2012年第45期4303-4305,共3页China Pharmacy

摘　　要：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。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.

关 键 词：氢溴酸西酞普兰 原料药 顶空气相色谱法 残留溶剂 测定 

分 类 号：R927.2[医药卫生—药学]