天然产物研究与开发 ›› 2018, Vol. 30 ›› Issue (增刊1): 45-50.doi: 10.16333/j.1001-6880.2018.S.008

• 研究论文 • 上一篇    下一篇

基于液质联用分析方法对酸枣仁中欧鼠李叶碱(Frangufoline)提取方法的研究

胡彦周,丁轲*,韩涛,陈湘宁   

  1. 北京农学院食品科学与工程学院 食品质量与安全北京实验室 农产品有害微生物及农残安全检测与控制北京市重点实验室,北京 102206  
  • 出版日期:2018-07-31 发布日期:2018-07-31
  • 基金资助:

    北京市属高等学校高层次人才引进与培养计划(CIT& CD20154045);北京市自然科学基金委员会—北京市教育委员会联合资助项目(KZ201710020014);北京农学院青年基金—实验技术体系研发基金(SXST201604)

     

Extraction of Frangufoline from Semen Zizyphi Spinosae by High Performance Liquid Chromatography-tandem Mass Spectrometry

HU Yan-zhou, DING Ke*, HAN Tao, CHEN Xiang-ning   

  1. College of Food Science and Engineering,Beijing Laboratory of Food Quality and Safety,Beijing University of Agriculture,Beijing 102206,China; Beijing Key Laboratory of Detection and Control of Spoilage Microorganisms and Pesticide Residues in Agricultural Products,Beijing 102206,China  
  • Online:2018-07-31 Published:2018-07-31

摘要: 建立酸枣仁中欧鼠李叶碱(酸枣仁碱A)的高效液相色谱-三重四极杆质谱分析方法,在此基础上,以酸枣仁为原料,以欧鼠李叶碱的提取率为考察指标,通过单因素试验和正交试验对酸枣仁中欧鼠李叶碱回流提取过程中的提取溶剂、提取溶剂中的酸、提取温度、酸浓度、液固比和提取时间进行优化,确定了乙醇为理想提取溶剂,提取溶剂中添加乙酸,最优回流提取工艺条件为:提取温度60 ℃,液固比20:1 (V∶g),乙酸浓度8%,提取时间4 h。最优提取工艺条件下欧鼠李叶碱的提取率为32.286 μg/g。

关键词: 酸枣仁, 欧鼠李叶碱, 高效液相色谱-串联质谱, 正交试验

Abstract: A sensitive high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of frangufoline (sanjoinine A) from Semen Zizyphi Spinosae.The reflux extraction conditions (extraction solvent,the acid in extraction solvent,extraction temperature,acid concentration,liquid-solid ratio,extraction time) of frangufoline from Semen Zizyphi Spinosae were investigated by single factor tests and orthogonal experiment with the extraction rate of frangufoline as the index.The results showed that the optimal extraction solvent was ethanol and the optimal acid was acetic acid.The optimal extraction conditions were as follows:extraction temperature 60 ℃,liquid-solid ratio 20∶1 (V∶g),acetic acid concentration 8%,extraction time 4 h.Under the optimal extraction conditions,the extraction rate of frangufoline was 32.286 μg/g.

Key words: Semen Zizyphi Spinosae, frangufoline, HPLC-MS/MS, orthogonal experiment

中图分类号: 

R284.2 O657.63