SCX-SPE结合UHPLC-Q-Exactive Orbitrap MS分析草乌中的四类二萜生物碱  

Identification of Four Diterpenoid Alkaloids in Radix Aconiti Kusnezoffii by SCX-SPE Combined with UHPLC-Q-Exactive Orbitrap MS

作　　者：周红燕 徐静 崔议方 宋书祎 兰先明 汪冰 张加余[1,2] Zhou Hongyan;Xu Jing;Cui Yifang;Song Shuyi;Lan Xianming;Wang Bing;Zhang Jiayu(School of Pharmacy,Shandong University of Traditional Chinese Medicine,Ji'nan 250300,China;School of Pharmacy,Binzhou Medical University,Yantai 264003,China;Shandong Institutes of Food and Drug Control,Ji'nan 250101,China)

机构地区：[1]山东中医药大学药学院,济南250300 [2]滨州医学院药学院,烟台264003 [3]山东省食品药品检验研究院,济南250101

出　　处：《世界科学技术-中医药现代化》2023年第7期2574-2585,共12页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：山东省教育厅人才引育项目(10073004):中药复杂体系作用模式解析创新研究团队,负责人:张加余;山东省组织部人才引育项目(tsqn202103110):泰山学者青年专家,负责人:张加余;山东省科学技术厅省重大科技创新工程项目(2021CXGC010511):中药配方颗粒质量识别与控制关键技术研究及产业化应用,负责人:林永强。

摘　　要：目的对草乌中的二萜生物碱进行表征分析。方法以强酸性阳离子交换树脂固相萃取(SCX-SPE)分离纯化草乌中的二萜生物碱,并结合超高效液相色谱串联四极杆静电场轨道阱质谱(UHPLC-Q-Exactive Orbitrap MS)进行结构鉴定。结果结合精确分子质量、多级质谱裂解规律、对照品对比、Clog P值及文献报道,共从草乌中鉴定了99个二萜生物碱类成分,包括双酯型二萜生物碱(DDA)27个,单酯型二萜生物碱(MDA)29个,酰胺型二萜生物碱(ADA)40个,多酯型二萜生物碱(PDA)2个,以及长链型二萜生物碱(LDA)1个。结论本文所建立的SCX-SPE结合UHPLC-Q-Exactive Orbitrap MS方法能快速地鉴定草乌中的二萜生物碱类成分,可为草乌的药效物质基础及质量控制研究提供科学依据。Objective To comprehensively characterize the diterpene alkaloids in Radix Aconiti Kusnezoffii.Methods The diterpene alkaloids were isolated and purified by strong acid cation exchange resin solid phase extraction column(SCX-SPE),and identified by ultra high performance liquid chromatography-Q-Exactive Orbitrap mass spectrometry(UHPLC-Q-Exactive Orbitrap MS).Results A total of 99 diterpene alkaloids were identified from Radix Aconiti Kusnezoffii,including 27 diester diterpene alkaloids(DDA),29 monoester diterpene alkaloids(MDA),40 amide diterpene alkaloids(ADA),2 polyester diterpene alkaloids(PDA)and 1 long-chain ester diterpene alkaloid(LDA).Conclusion The SCX-SPE combined with UHPLC-Q-Exactive Orbitrap MS method,established in this paper,can rapidly identify a large number of diterpene alkaloids in Radix Aconiti Kusnezoffii,which provides scientific proof for the study of pharmacodynamic substance basis and quality control of Radix Aconiti Kusnezoffii.

关 键 词：草乌 二萜生物碱 强酸性阳离子交换树脂固相萃取柱(SXC-SPE) 超高效液相色谱-串联四极杆静电场轨道阱质谱(UHPLC-Q-Exactive Orbitrap MS) 

分 类 号：R284.1[医药卫生—中药学]