基于UPLC-Q-TOF-MS/MS技术的布渣叶化学成分分析  

Analysis of Chemical Constituents in Microctis Folium by UPLC-Q-TOF-MS/MS

作　　者：肖观林 江洁怡 李素梅 陈伟韬 陈昭 张靖年 毕晓黎 XIAO Guan-lin;JIANG Jie-yi;LI Su-mei;CHEN Wei-tao;CHEN Zhao;ZHANG Jing-nian;BI Xiao-li(Guangdong Provincial Key Laboratory of Research and Development in Traditional Chinese Medicine(TCM),Guangdong Province Engineering Technology Research Institute of TCM,Guangzhou 510095,China)

机构地区：[1]广东省中医药工程技术研究院,广东省中医药研究开发重点实验室,广州510095

出　　处：《中国实验方剂学杂志》2021年第3期138-148,共11页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家“重大新药创制”科技重大专项(2018ZX09301011-002);广东省科技计划项目(2017A070701017)。

摘　　要：目的:应用超高效液相色谱-四级杆-飞行时间高分辨质谱法(UPLC-Q-TOF-MS/MS)分析布渣叶中的化学成分。方法:色谱条件为Waters CORTECS UPLC C18色谱柱(2.1 mm×150 mm,1.6μm),以甲醇(A)-0.1%甲酸水溶液(B)流动相进行梯度洗脱(0~4 min,14%~30%A;4~16 min,30%~58%A;16~25 min,58%~78%A;25~25.1 min,78%~98%A;25.1~29 min,98%A),流速0.25 mL·min^(-1),进样量1μL;质谱条件为电喷雾离子源(ESI),在正、负离子模式下对色谱流出物进行检测,检测范围m/z 100~1 500。结果:通过高分辨质谱数据分析、结合参考文献数据以及对照品确认,从布渣叶中共鉴别出31个化学成分,包括28个黄酮类(9个黄酮碳苷类,10个黄酮醇及其苷类,8个原花青素类,1个苯骈色原酮类)和3个有机酸类(咖啡酸、阿魏酸和p-香豆酸)。结论:UPLC-Q-TOF-MS/MS技术为鉴别布渣叶药材中化学成分提供简便、快速、准确的方法,其主要化学成分为黄酮碳苷类、黄酮醇氧苷类、原花青素类,7个原花青素类成分在该植物中属首次发现,可为布渣叶药材的质量评价及药效物质基础研究提供参考。Objective:To analyze the chemical constituents in Microctis Folium by ultra performance liquid chromatography-quadrupole-time-of-flight high resolution mass spectrometry(UPLC-Q-TOF-MS/MS).Method: Waters CORTECS UPLC C18 column(2.1 mm×150 mm,1.6 μm)was used for chromatographic separation with the mobile phase of methanol(A)-0.1% formic acid solution(B)for gradient elution(0-4 min,14%-30%A;4-16 min, 30%-58%A;16-25 min, 58%-78%A;25-25.1 min, 78%-98%A;25.1-29 min,98%A),the flow rate was 0.25 mL· min^(-1),the injection volume was 1 μL. The electrospray ionization(ESI)was adopted for determining the chromatographic effluent under positive and negative ion modes,the main chromatographic peaks were assigned and distinguished by Q-TOF,and the scanning range was m/z 100-1 500.Result: A total of 31 chemical constituents in Microctis Folium were identified by confirmation of reference substances,literature comparison and high resolution mass spectrometry data analysis. The chemical constituent cluster was composed of 28 flavonoids(9 flavone C-glycosides, 10 flavonols and their glycosides, 8 proanthocyanidins,1 xanthone)and 3 organic acids(caffeic acid,p-coumaric acid,ferulic acid). Conclusion:UPLC-Q-TOF-MS/MS technique provides a simple,rapid and accurate method for the identification of chemical constituents in Microctis Folium. Flavone C-glycosides,flavonol oxyglycosides and proanthocyanidins are the main chemical constituents. The 7 proanthocyanidins are reported for the first time in this herb. In conclusion,the chemical profile of Microctis Folium is characterized and the findings are meaningful for the in-depth quality assessment and material basis clarification of Microctis Folium.

关 键 词：布渣叶 超高效液相色谱-四级杆-飞行时间高分辨质谱法(UPLC-Q-TOF-MS/MS) 化学成分 黄酮碳苷类 黄酮醇氧苷类 原花青素类 有机酸类 

分 类 号：R22[医药卫生—中医基础理论] R28[医药卫生—中医学]