基于UPLC-Q-Orbitrap HRMS益智仁中倍半萜类物质的分析与鉴定  

Analysis and Identification of Sesquiterpenes in Alpinia oxzphylla Miq Based on UPLC-Q-Orbitrap HRMS

作　　者：张梦雅 左莉华[1,2] 周霖 高一乔[1,2] 关克磊 杜翔宇 张瑞[1,2] 贾清泉 裴健颖 李寒冰[4] 孙志 杜书章[1,2] ZHANG Meng-ya;ZUO Li-hua;ZHOU Lin;GAO Yi-qiao;GUAN Ke-lei;DU Xiang-yu;ZHANG Rui;JIA Qing-quan;PEI Jian-ying;LI Han-bing;SUN Zhi;DU Shu-zhang(Department of Pharmacy,the First Affiliated Hospital of Zhengzhou University,Zhengzhou 450052,China;Henan Key Laboratory of Precision Clinical Pharmacy,Zhengzhou 450052,China;School of Basic Medical Sciences,Henan University,Kaifeng 475000,China;College of Pharmacy,Henan University of Chinese Medicine,Zhengzhou 450052,China)

机构地区：[1]郑州大学第一附属医院药学部,河南郑州450052 [2]河南省精准临床药学重点实验室,河南郑州450052 [3]河南大学基础医学院,河南开封475000 [4]河南中医药大学药学院,河南郑州450052

出　　处：《中草药》2020年第24期6168-6177,共10页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(81703666);国家自然科学基金资助项目(82003921);河南省高等学校重点科研项目基础研究计划(19A360008);河南省高等学校重点科研项目基础研究计划(19A320070);河南省科技计划项目(182102310243)。

摘　　要：目的建立中药复杂体系快速、准确鉴定的分析方法,系统阐明益智仁(益智Alpinia oxyphylla的干燥成熟果实)中倍半萜类物质的化学组成。方法采用超高效液相色谱-四级杆/静电场轨道阱高分辨质谱(UPLC-Q-Orbitrap HRMS)技术,在优化倍半萜类物质提取工艺的基础上,通过质谱全扫描捕捉未知化合物的精确相对分子质量及二级碎片离子信息,同时与对照品的相对保留时间和质谱数据进行比对,并结合相关参考文献及数据库,实现对益智仁中倍半萜类未知化合物的准确快速鉴定。结果共鉴定出24种倍半萜类化合物,根据骨架结构将其归为4类,其中9个桉叶烷型、6个杜松烷型、8个艾里莫芬烷型、1个刺参酮型。结论利用所建立的分析方法,实现对益智仁中多种倍半萜类成分的快速、准确鉴定,为益智仁药效物质基础及质量控制研究提供理论依据。Objective To establish a rapid and accurate analytical method for the identification of complex system of traditional Chinese medicine, and to systematically clarify the chemical composition of sesquiterpenes in Alpinia oxyphylla. Method On the basis of optimizing the extraction process of sesquiterpenes, the accurate molecular weight and secondary fragment ions information of unknown compounds were captured by ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry(UHPLC-Q-Orbitrap HRMS). Compared with the relative retention time and mass spectrometry data of the reference substance, combined with relevant references and databases, the sesquiterpene unknown compounds in the fruits of A. oxyphylla were accurately and rapidly characterized. Results A total of 24 sesquiterpenes were identified and classified into four categories according to their skeleton structure, including nine eudesmane-type, six cadinane-type, eight eremophilane-type, and one oplopanone-type. Conclusion In this study, the established analytical method was used to realize the rapid and accurate identification of sesquiterpenes in the fruits of A. oxyphylla, which provided a theoretical basis for the research on the pharmacodynamic substance basis and quality control of the fruits of A. oxyphylla.

关 键 词：益智仁 倍半萜类 超高效液相色谱-四级杆/静电场轨道阱高分辨质谱 提取工艺 桉叶烷型 杜松烷型 

分 类 号：R284.1[医药卫生—中药学]