基于UPLC-Q-TOF-MS的布芍调脂胶囊化学成分分析

目的:采用超高效液相色谱-四级杆-飞行时间串联质谱(UPLC-Q-TOF-MS)技术对中药复方布芍调脂胶囊中的化学成分进行定性分析。方法:采用Waters CORTECS UPLC C18色谱柱(2.1 mm×150 mm,1.6μm),流动相甲醇-0.1%甲酸水溶液进行梯度洗脱,柱温40℃,流速0.24 mL·min^-1,进样量1μL;质谱条件为X500R QTOF质谱仪,电喷雾离子源(ESI)分别在正、负离子模式下对色谱流出物进行高分辨四极杆飞行时间串联质谱检测,对各主要色谱峰进行归属。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,共鉴别出53个化学成分,包括21个黄酮类,10个酚酸类,5个单萜及其苷类,7个二萜内酯类及10个倍半萜类成分,并对化合物的药材来源进行了归属,其中5个黄酮类化合物(芒果苷、异槲皮苷、香蒲新苷、异鼠李素-3-O-新橙皮苷、银椴苷)首次在布渣叶中发现。结论:UPLC-Q-TOF-MS联用技术为鉴别布芍调脂胶囊中化学成分提供简便、快速、准确的方法,鉴定得到的各类化学成分基本可涵盖组方中各药材的主要成分,为进一步阐明布芍调脂胶囊的药效物质基础、作用机制及优选质量控制指标提供了理论依据和技术方法。

Analysis of Chemical Constituents in Bushao Tiaozhi Capsules by UPLC-Q-TOF-MS

Objective:To analyze the main chemical constituents of traditional Chinese medicine compound Bushao Tiaozhi capsules by using UPLC-Q-TOF-MS technology.Method:The separation was eluted with Waters CORTECS UPLC C18 column(2.1 mm×150 mm,1.6μm)in a gradient mode,with methanol-0.1%formic acid as the mobile phase.The column temperature was 40℃,the flow rate was 0.24 mL·min^-1,and the injection volume was 1μL.The mass spectrometry condition was X500R QTOF mass spectrometry,the positive and negative electrospray ionization(ESI)was adopted for determine the chromatographic effluent,and the main chromatographic peaks were assigned and distinguished by Q-TOF.Result:A total of 53 chemical constituents were identified by reference confirmation,literature comparison,and high mass spectrometry data analysis.The chemical constituent cluster was composed of 21 flavonoids,10 phenolics,5 monoterpene glycosides,7 diterpene lactones and 10 sesquiterpenes.Furthermore,all of the constituents were surveyed and classified according to their medicinal materials derivation.Among them,the 5 flavonoids components(mangiferin,isoquercitrin,typhaneoside,isorhamnetin 3-O-neohesperidoside,tiliroside)were identified in Microctis Folium for the first time.Conclusion:This study shows that UPLC-Q-TOF-MS technology provides a simple,rapid,and accurate method for the identification of chemical constituents in Bushao Tiaozhi capsules.The identified chemical components mostly cover the main constituents of each medicinal material in the formula,so as to provide a new technological method and theoretical foundation for further defining the pharmacological basis and mechanism of action and optimizing the quality control of Bushao Tiaozhi capsules.