顶空气相色谱法测定盐酸司他斯汀中6种残留溶剂  

Determination of six residual organic solvents in setastine hydrochloride by headspace gas chromatography

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)

机构地区：[1]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌330029

出　　处：《分析试验室》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。

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.

关 键 词：盐酸司他斯汀 残留溶剂 顶空气相色谱法 

分 类 号：TQ460.7[化学工程—制药化工] R917[医药卫生—药物分析学]