琥珀酸多西拉敏有机溶剂残留量测定的方法  

Determination of residual organic solvents in doxylamine succinate by gas chromatography

作　　者：乔乔 余小红 许龙[1] 李娟 曹阳 曹明成[1] 黄顺旺 QIAO Qiao;YU Xiaohong;XU Long;LI Juan;CAO Yang;CAO Mingcheng;HUANG Shunwang(Author Affiliation:Hefei Innovative Pharmaceutical Technology Co.,Ltd.,Hefei,Anhui 230088,China)

机构地区：[1]合肥创新医药技术有限公司,安徽合肥230088

出　　处：《安徽医药》2020年第9期1729-1731,共3页Anhui Medical and Pharmaceutical Journal

基　　金：合肥市2018年省战略性新兴产业集聚发展基地研发类项目(11)。

摘　　要：目的建立琥珀酸多西拉敏原料中8种有机溶剂残留量的测定方法。方法采用毛细管气相色谱法,色谱柱为ZBWAX Plus毛细管柱(以聚乙二醇为固定相),配备FID检测器,程序升温,载气为氮气,70%二甲基亚砜为溶剂,以外标法定量检测琥珀酸多西拉敏原料药中的甲基叔丁基醚、四氢呋喃、乙酸乙酯、异丙醇、乙苯、对二甲苯、间二甲苯和邻二甲苯的残留量。结果在所建立的色谱条件下,8种有机溶剂完全分离,在所考察的浓度范围内具有良好线性,r为0.999 0~0.999 5,平均回收率99.1%~101.6%,精密度相对标准偏差(RSD)均小于10%。结论本方法操作简便,能够准确测定琥珀酸多西拉敏的有机溶剂残留量。Objective To establish a method for determination of the eight residual organic solvents in doxylamine succinate.Methods The contents of methyl tert⁃butyl ether,tetrahydrofuran,ethyl acetate,isopropanol,ethylbenzene,p⁃xylene,m⁃xylene and o⁃xylene in doxylamine succinate were quantitatively detected by external standard method.The capillary gas chromatography was performed on a ZB⁃WAX Plus(polyethyleneglycol as the stationary phase)capillary column,with FID detector,temperature pro⁃grammed,with nitrogen as carrier gas and 70%DMSO as solvent.Results Under the established chromatographic conditions,the eight residual organic solvents of doxylamine succinate were separated efficiently by GC,with good the linearity within the observed concentration range,and the regression coefficient were in the range from 0.9990 to 0.9995,respectively,while the recoveries were in the range from 99.1%to 101.6%,and the RSD of precision were all less than 10%.Conclusion This method is simple,and it can be used to accurately determinate the residual organic solvents contend in doxylamine succinate.

关 键 词：多西拉敏/分析 色谱法 气相 溶剂 有机化学品 有机溶剂残留量 

分 类 号：R927.2[医药卫生—药学]