摘要
目的:建立超高效液相色谱-四极杆-静电场轨道阱质谱(UHPLC-Q-Exactive Orbitrap MS)法对附子中二萜类生物碱成分进行全面分析表征。方法:首先采用强阳离子交换树脂-固相萃取(SCX-SPE)柱纯化富集附子二萜类生物碱,并采用兼顾高分离度、高专属性和高分辨率的UHPLC-Q-Exactive Orbitrap MS对其进行全面鉴定分析。结果:结合色谱保留行为、精确相对分子质量、多级质谱裂解规律、对照品比对以及文献报道等,共从附子提取物中鉴定了101个二萜生物碱,包括双酯型(DDA)14个、单酯型(MDA)29个、酰胺型(ADA)57个及多酯型(PDA)1个。结论:本研究全面表征了附子二萜类生物碱,可为其相关作用机制和开发利用研究提供参考依据。
Objective:To establish a method for rapid identification of diterpenoid alkaloids in Aconitum carmichaeli Debx.by ultrahigh performance liquid chromatography-quadruple orbitrap tandem mass spectrometry(UHPLC-Q-Exactive Orbitrap MS).Methods:In this paper,solid phase extraction column with strong cation exchange-solid phase extraction(SCX-SPE)was used to purify and enrich aconite diterpenoid alkaloids.And UHPLC-Q-Exactive Orbitrap MS with high separation,specificity and resolution was used for comprehensive identification and analysis.Results:Combined with chromatographic retention behavior,accurate molecular weight,multistage mass spectrometry pyrolysis,comparison of reference substances and literature reports,a total of 101 diterpenoid alkaloids were identified from the extract of Aconitum carmichaeli Debx.,including 14 diester diterpene alkaloids(DDA),29 alcoholamine diterpene alkaloids(MDA),57 alcoholamine diterpene alkaloids(ADA)and 1 polyester type diterpene alkaloid(PDA).Conclusion:This study comprehensively characterized the diterpenoid alkaloids of Aconitum carmichaeli Debx.,which can provide a reference for their related mechanism and development and utilization research.
作者
宋书祎
兰先明
徐静
崔议方
周红燕
郑健
戴胜云
张加余
SONG Shu-yi;LAN Xian-ming;XU Jing;CUI Yi-fang;ZHOU Hong-yan;ZHENG Jian;DAI Sheng-yunn;ZHANG Jia-yu(School of Pharmacy,Binzhou Medical University,Yantai 264003,China;School of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250300,China;National Institutes for Food and Drug Control,Beijing 102629,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2023年第6期918-929,共12页
Chinese Journal of Pharmaceutical Analysis
基金
山东省泰山学者青年专家项目(tsqn202103110)
山东省中药材及饮片标准研究课题(2020-246)
山东省青创人才引育团队——中药复杂体系作用模式解析创新研究团队(10073004)
中国食品药品检定研究院中青年基金资助项目——基于多源数据融合的乌头属毒性药材鉴别方法研究(2022A2)
山东省重大科技创新工程项目——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(2021CXGC010511)。
