摘要
本文提出了用气相色谱法测定琥珀酸曲格列汀原料药中6种残留溶剂的方法。采用毛细管色谱柱DB-624(30 m×0.32 mm×1.8μm)、程序升温方式,载气为N 2,检测器为氢火焰离子化检测器,分流比为10∶1。方法学验证结果表明残留溶剂乙醇、异丙醇、乙酸乙酯、二氯甲烷、四氢呋喃、N,N-二甲基甲酰胺可以很好分离,6种溶剂的平均回收率为96.40%~100.9%,检测限和定量限远远低于“人用药品注册技术要求国际协调会议”规定的限量浓度,方法的精密度与溶液稳定性均满足测定要求。本方法可作为琥珀酸曲格列汀原料药中残留溶剂的有效测定方法。
In this papera new method was firstly proposed to determinesix residue organic solvent in trelagliptin succinate by gas chromatography.DB-624(30 m×0.32 mm×1.8μm)capillary column was adopted.Six residual organic solvents,i.e.ethanol,isopropanol,ethyl acetate,dichloromethane,tetrahydrofuran,N,N-dimethylformamide were separated and tested under a gradient temperature with nitrogen gas as carrier and FID as detector.The shunt ratio was 10∶1.The verification of methodology showed the six residual organic solvents could be separated effectively.The average recovery rates of six solvents were from 96.40%to100.9%,and the detection limits and quantitative limits were far below the limited concentrations prescribed by International Council for Harmonization(ICH).The precision of method and the stability of solution also indicated the studied method could be used to determine effectively the six residual organic solvents in trelagliptin succinate.
作者
龚爱琴
扈宁
钱琛
金党琴
GONG Ai-qin;HU Ning;QIAN Chen;JIN Dang-qin(Yangzhou Polytechnic Institute,Yangzhou 225127,China;West China School of Stomatology,Sichuan University,Chengdu 610000,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2020年第10期1934-1938,共5页
Chemical Research and Application
基金
江苏高校“青蓝工程”项目(苏教师[2018]12号)资助
江苏省高等学校优秀科技创新团队项目(苏教科[2017]6号)资助。
关键词
琥珀酸曲格列汀
残留溶剂
气相色谱法
trelagliptin succinate
residual organic solvent
gas chromatography
