超高效液相串联质谱快速定性分析大蓟  

A Rapid Ultraperformance Liquid Chromatography-tandem Mass Spectrometric Method for Qualitative Analysis of Cirsium japonicum

作　　者：彭海博 吴霞[1] 张宇[1] 冯毅凡[1] 

机构地区：[1]广东药学院中心实验室,广东广州510000

出　　处：《亚太传统医药》2015年第2期16-19,共4页Asia-Pacific Traditional Medicine

基　　金：国家自然科学基金项目(1035102201000000);教育部广东工业大学合作研究项目(2009B090300349;2011B090400379)

摘　　要：大蓟是治疗高血压、各种出血和炎症的一种中药,但目前鲜有关于其有效成分的报道。通过UPLC/Q-TOF建立一种快速高效的方法对大蓟所含成分进行分析。基于精确分子量、计算分子成分,结合二级质谱数据及相关文献报道,发现并确定29种成分结构,包括黄酮、黄酮糖苷、异黄酮、有机酸和蒽醌类化合物。其中斑鸠菊酸、叔丁基羟基茴香醚、二氢辣椒素、大黄蒽醌和紫杉叶素等为首次在大蓟中发现并讨论其ESI源中的二级质谱裂解规律,黄酮在ESI源中脱去CO和H2O的二级裂解规律也初次被阐述。Cirsium japonicum is a perennial medicinal plant. A better understanding of this herb requires the detection of new poten- tially useful compounds and analysis of their application. A rapid and sensitive method for identification of the constituents of C. ja ponicum was developed, which employed ultraperformance liquid chromatography coupled with electrospray ionization-tandem qua- drnpole high resolution time-of-flight mass spectrometry （UPLC/Q-TOF MS）. Using this approach, 29 compounds were identified and tentatively characterized, in a period of 17min. These compounds included flavonoids, flavone glycosides, isoflavonoids, organic acids, phenolic acids, and anthraqninones. Among them, vernolic acid, butylated hydroxyanisole, physeion, and taxifolin have been reported for C. japonicum for the first time, and their fragmentation behavior upon electrospray ionization has been discussed. Unu sual H2 O and CO loss in flavonoids was characterized here for the first time and a new diagnostic ion and new fragmentation pattern were proposed for dihydroeapsaicin. The results indicated that UPLC/Q-TOF MS was a powerful complementary tool for structural characterization by ESI MS/MS.

关 键 词：大蓟 二级质谱碎片 超高效液相-Q-TOF-MS 快速分析 

分 类 号：R284.1[医药卫生—中药学]