摘要
建立了顶空气相色谱法(HS-GC)测定盐酸司他斯汀中乙醚、丙酮、异丙醇、四氢呋喃、甲苯与二甲苯6种有机溶剂残留量的方法。样品用二甲基亚砜溶解,在110℃加热20 min,使气液平衡,采用氢火焰离子化检测器(FID),以DB-1701(60 m×0.320 mm,1.00μm)为分析柱,程序升温测定。在优化的气相色谱条件下,6种残留溶剂均能有效分离,在考察浓度范围内,线性关系良好(R^(2)=0.9998~1.0000),平均回收率96.5%~98.9%(n=9)。方法适用于盐酸司他斯汀中残留溶剂的日常检测。
A headspace gas chromatography(HS-GC)method was established for the determination of six residual solvents including ethyl ether,acetone,isopropanol,tetrahydrofuran,toluene and xylene in setastine hydrochloride.The sample was dissolved in dimethyl sulfoxide,heated at 110℃for 20 minutes in order to reach the vaporliquid equilibrium state,and detected by flame ionization detector(FID).DB-1701 capillary column(60 m×0.320 mm,1.00μm)was used with the column temperature raised by program.Under optimized conditions of HS-GC,the six residual organic solvents were separated well.Good linearities were obtained in the experimental concentration(correlation coefficient:R^(2)=0.9998-1.0000).The average recoveries were in the range from 96.5%to 98.9%(n=9).The method is suitable for the routine detection of the six residual solvents in setastine hydrochloride.
作者
夏红英
钟振华
余师师
裴昆
刘贞
程奇珍
XIA Hongying;ZHONG Zhenhua;YU Shishi;PEI Kun;LIU Zhen;CHENG Qizhen(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Dmg and Medical Device Quality,Nanchang 330029)
出处
《分析试验室》
CAS
CSCD
北大核心
2021年第1期70-74,共5页
Chinese Journal of Analysis Laboratory
基金
江西省药品监督管理局科研项目(2019JS06)
国家药品标准提高研究项目(药典综〔2018〕482号,2018H093)资助。
关键词
盐酸司他斯汀
残留溶剂
顶空气相色谱法
setastine hydrochloride
residual organic solvents
headspace gas chromatography
