•  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
热点追踪
期刊检索


检索
检索项:
检索词:
总目录
  • WCSB9︱2019(第九届)世界采样和混样大会 查看全文>>
  • 关于召开第十五届全国青年分析测试学术报告会的通知 查看全文>>
友情链接
DOLPA/AOT-异辛烷反胶束萃取-UPLC法测定倒提壶中4种生物碱的含量
    点此下载全文
作者单位
樊轻亚,王万好,代春美 1.信阳职业技术学院
2.河南同源制药有限公司
3.中国中医科学院 
基金项目:河南省科技厅科技攻关项目(172102310315);信阳职业技术学院青年骨干教师培训计划
中文摘要:建立了二(2-乙基己基)磷酸酯(DOLPA)/ 二(2-乙基己基)丁二酸酯磺酸钠(AOT)-异辛烷反胶束萃取技术结合超高效液相色谱同时测定倒提壶中天芥菜品、天芥菜碱、毛果天芥菜碱及天芥菜定含量的方法。采用单因素试验考察了表面活性剂的种类与浓度、水相pH值、盐的种类与浓度、萃取相比、萃取及反萃取时间等因素对生物碱萃取率的影响。确定最佳萃取条件为:DOLPA/AOT的总浓度为0.6 mol/L,水相pH值为4.0,KCl浓度为0.2 mol/L,萃取相比4∶1,萃取和反萃取时间分别为 10、30 min。在优化条件下,以乙腈-0.2%三乙胺为流动相进行超高效液相色谱法(UPLC)梯度洗脱,可在 16 min 内完成色谱分析,4种生物碱色谱峰的分离度良好;天芥菜品、天芥菜碱、毛果天芥菜碱及天芥菜定4种生物碱的质量浓度与峰面积呈良好线性关系,检出限分别为0.030、0.050、0.040、0.020 mg/L,回收率分别为98.2%~103%、97.9%~102%、98.1%~101%、97.8%~104%,精密度、重复性及加标回收率的RSD 均不大于 2.3%。该法简单快捷、灵敏准确,满足倒提壶中4种生物碱的检测要求。
中文关键词:倒提壶  生物碱  反胶束  超高效液相色谱法(UPLC)
 
Determination of Four Alkaloids in Cynoglossum Amabile Stapf et Drumm by Ultrahigh Performance Liquid Chromatography with DOLPA/AOT-Isooctane Reverse Micelles Extraction
Abstract:A method of ultrahigh performance liquid chromatography(UPLC) with DOLPA/AOT-isooctane reverse micelles was developed for the determination of heliosupine,heliotrine,lasiocarpine and heliotridine in Cynoglossum amabile Stapf et Drumm.Experimental conditions affecting the reverse micelles such as types and concentration of surface active agent,pH value,salt species and concentration,ratio of sample and reverse micelles,extraction time and back extraction time were optimized.The optimal conditions were as follows:DOLPA /AOT concentration:06 mol/L,pH value:40,KCl concentration:02 mol/L,ratio of sample and reverse micelles:4∶1,extraction time:10 min,back extraction time:30 min.Under the optimal conditions,heliosupine,heliotrine,lasiocarpine and heliotridine were separated,and determined by UPLC with acetonitrile-02% triethylamine as mobile phase by gradient elution.Four ingredients were separated in 16 min.There existed good linear relationships for the analytes between peak areas and concentrations,with detection limits of 0030,0050,0040 and 0020 mg/L,respectively.The recoveries were in the ranges of 982%-103%,979%-102%,981%-101% and 978%-104%,respectively.The RSDs for recovery,precision and reproducibility were not more than 23%.The method is convenient,sensitive and accurate,and is suitable for the determination and confirmation of 4 alkaloid in Cynoglossum amabile Stapf et Drumm.
Key Words:Cynoglossum amabile Stapf et Drumm  alkaloids  reverse micelles  ultrahigh performance liquid chromatography(UPLC)
引用本文:樊轻亚,王万好,代春美.DOLPA/AOT-异辛烷反胶束萃取-UPLC法测定倒提壶中4种生物碱的含量[J].分析测试学报,2018,37(12):1445-1450.
摘要点击次数: 27
全文下载次数: 35
查看全文  查看/发表评论  下载PDF阅读器