基于UHPLC-Q-Exactive-MS技术的短序蒲桃叶岩白菜素新衍生物的快速发现  

Rapid Identification of New Bergenin Derivatives in Syzygium Brachythyrsum Based on Ultrahigh Performance Liquid Chromatography-Q-Exactive Orbitrap Mass Spectrometry

作　　者：涂海声 邱嘉琦 徐雅 张靖 丘小惠 黄志海 李钟 徐文 韩彬 TU Hai-sheng;QIU Jia-qi;XU Ya;ZHANG Jing;QIU Xiao-hui;HUANG Zhi-hai;LI Zhong;XU Wen;HAN Bin(Guangdong Pharmaceutical University,School of Traditional Chinese Medicine,Guangzhou 510006,China;The Second Clinical College of Guangzhou University of Chinese Medicine,Guangdong Provincial Hospital of Chinese Medicine,Guangzhou 510006,China;Guangzhou Key Laboratory of Chirality Research on Active Components of Traditional Medicine,Guangzhou 510006,China)

机构地区：[1]广东药科大学中药学院,广东广州510006 [2]广州中医药大学第二附属医院,广东省中医院,广东广州510006 [3]广州市中药活性成分手性研究重点实验室,广东广州510006

出　　处：《分析测试学报》2022年第7期988-997,共10页Journal of Instrumental Analysis

基　　金：青年科学基金项目(81803482);广州市重点实验室建设项目(202002010004)。

摘　　要：基于课题组前期对短序蒲桃叶的研究,该文建立了快速鉴定短序蒲桃叶中未知岩白菜素类化学成分的超高效液相色谱-串联四极杆轨道阱质谱(UHPLC-Q-Exactive-MS)分析方法。采用Waters ACQUITY UPLC HSS T3色谱柱(1.8μm,2.1 mm×100 mm),乙腈-0.1%甲酸水为流动相梯度洗脱,Orbitrap MS负离子模式下检测。总结了模式成分的质谱裂解规律和特征碎片离子,并采集高分辨质谱数据对短序蒲桃叶中的岩白菜素衍生物等酚酸类成分进行鉴定。从短序蒲桃叶中鉴定出54种酚酸类成分,包含34种岩白菜素衍生物,均为在蒲桃属植物中首次报道,其中发现潜在的新岩白菜素类化合物10个。所得结果为进一步研究和利用民族中草药短序蒲桃提供了参考。Plants from the genus Syzygium have significant medicinal and edible application values.Syzygium brachythyrsum(S.brachythyrsum)has been widely used as a traditional ethnic Chinese medicine in southwest China.However,the knowledge about its chemical compositions and pharmacological effects is still unknown.Several new bergenins derivatives from this medicinal plant were isolated for the first time in the previous study.In the present work,a rapid and effective method was established for the identification and characterization of bergenins derivatives in S.brachythyrsum based on ultrahigh performance liquid chromatography-Q-exactive orbitrap mass spectrometry(UHPLC-Q-Exactive-MS).The methanol extract of S.brachythyrsum was separated on a Waters ACQUITY UPLC HSS T3 column(1.8μm,2.1 mm×100 mm),using acetonitrile-water containing 0.1%formic acid as mobile phase,then detected by UHPLC-Q-Exactive-MS in negative mode.Based on the combination of the high-resolution mass determination,the fragmentation behaviors and fragmentation pattern of model compounds,and diagnostic fragment ions filtering strategy,54 compounds including 34 bergenins derivatives were identified or tentatively characterized from S.brachythyrsum.These bergenins derivatives mainly composed of O-galloyl,feruloyl,sinapoyl,coumaroyl,syringyl,caffeoyl,and hydroxy benzoyl substituted bergenins and norbergenins.Furthermore,a series of hexahydroxydiphenoyl(HHDP)substituted bergenins were identified as potential new natural products.All these bergenin derivatives were found in the Syzygium genus for the first time.The results of this paper demonstrated for the first time that S.brachythyrsum is a rich resource of bergenin derivatives,and it provides a reference for further research and utilization of Chinese herbal medicine S.brachythyrsum.

关 键 词：蒲桃属 短序蒲桃 液相色谱-质谱(LC-MS) 岩白菜素 

分 类 号：O657.63[理学—分析化学] R914.1[理学—化学]