双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱

樊轻亚; 许卫军; 代春美

doi:doi：10.3969/j.issn.1004-4957.2019.11.007

您当前的位置：

首页 >

文章列表页 >

双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱

- 双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱
- Determination of Eight Alkaloids in Cynoglossum amabile Stapf et Drumm by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Aqueous Two phase Extraction
- 分析测试学报 2019年38卷第11期页码：1328-1334
- 作者机构：
  
  1. 信阳职业技术学院药学院
  2. 中国中医科学院
- 作者简介：
- 基金信息：
  
  河南省科技厅科技攻关项目(172102310315);第24批博士后科技服务团合作项目
- DOI：doi：10.3969/j.issn.1004-4957.2019.11.007
  中图分类号：
- 纸质出版：2019
- 稿件说明：
移动端阅览
樊轻亚, 许卫军, 代春美. 双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱[J]. 分析测试学报, 2019,38(11):1328-1334.

樊轻亚, 许卫军, 代春美. Determination of Eight Alkaloids in Cynoglossum amabile Stapf et Drumm by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Aqueous Two phase Extraction[J]. 2019, 38(11): 1328-1334.
樊轻亚, 许卫军, 代春美. 双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱[J]. 分析测试学报, 2019,38(11):1328-1334. DOI： doi：10.3969/j.issn.1004-4957.2019.11.007.

樊轻亚, 许卫军, 代春美. Determination of Eight Alkaloids in Cynoglossum amabile Stapf et Drumm by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Aqueous Two phase Extraction[J]. 2019, 38(11): 1328-1334. DOI： doi：10.3969/j.issn.1004-4957.2019.11.007.

摘要

建立了乙醇-磷酸氢二钾双水相萃取技术结合超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定倒提壶中8种生物碱含量的方法。采用单因素实验考察了双水相的萃取条件对倒提壶中8种生物碱萃取率的影响，最佳萃取条件为：乙醇质量分数为30%，K2HPO4·3H2O的质量分数为20%，萃取剂与样品相比为6∶1，水相的pH值为4.0。以乙腈-0.1 mol/L醋酸铵为流动相进行UHPLC-MS/MS分析，8种生物碱之间具有良好的分离度，各成分在一定质量浓度范围内具有良好的线性关系(r2＞0.99)。方法的精密度、重复性及加标回收率的相对标准偏差（RSD）均小于 3.0%。方法简单快捷、灵敏准确，可满足倒提壶中生物碱检测的要求。

Abstract

An ultrahigh performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) with EtOH/K2HPO4·3H2O aqueous two-phase extraction was developed for the simultaneous determination of eight alkaloids in Cynoglossum amabile Stapf et Drumm.Effects of aqueous two phase extraction conditions on extraction efficiencies of eight alkaloids were optimized by single factor experiment.The optimum conditions were as follows:30%(mass ratio) of ethanol

20%(mass ratio) of K2HPO4·3H2O

6∶1 for an extractant to sample ratio

and 4.0 for pH value.The extract was analyzed by UHPLC-MS/MS with acetonitrile-0.1 mol/L ammonium acetate as mobile phases

and eight alkaloids in the extract were well separated.There were good linear relationships for the analytes in the certain concentration ranges with their correlation coefficients(r2) larger than 0.99.The relative standard deviations(RSDs) for precision

reproducibility and recovery were all less than 3.0%.The method is convenient，sensitive and accurate，and is suitable for the determination and confirmation of eight alkaloids in Cynoglossum amabile Stapf et Drumm.

关键词

Keywords

references

浏览量

222

下载量

CSCD

文章被引用时，请邮件提醒。

提交

工具集

关联资源

基于液质联用技术的川贝母及其混伪品生物碱类成分差异研究

卡痛叶中生物碱类活性成分研究进展

分散固相萃取/超高效液相色谱－串联质谱法测定药用狗牙花中6种生物碱

垃圾焚烧厂周边土壤中微塑料质量丰度的Py/GC-MS和TD/GC-MS比较研究

纳塑料的超分辨光学成像研究进展