UHPLC-Q-Orbitrap HRMS鉴定丹灯通脑软胶囊中多种化学成分

Identification of Various Chemical Constituents in Dandeng Tongnao Capsule by UHPLC-Q-Orbitrap HRMS

关键词:  丹灯通脑软胶囊  超高效液相色谱-四级杆/静电场轨道阱高分辨质谱  化学成分分析

Key words:  dandeng tongnao capsule  UHPLC-Q-Orbitrap HRMS  chemical constituents analysis

摘要:

目的 应用超高效液相色谱-四级杆/静电场轨道阱高分辨质谱（UHPLC-Q-Orbitrap HRMS）对丹灯通脑胶囊中的化学成分进行快速分析鉴别。方法 采用ACQUITY UPLC^® BEH C₁₈色谱柱（2.1 mm×50 mm，1.7 μm），乙腈-0.1%甲酸水为流动相进行梯度洗脱，分离各个化学成分，质谱采用全扫描模式，正负离子同时扫描检测色谱流出物。根据质谱提供的化合物精准分子量、多级碎片离子信息，结合相关参考文献和数据库信息，同时与对照品的相对保留时间和质谱数据进行比对，定性鉴定化合物。结果 共鉴定出59种化学成分，主要包括黄酮类、醌类、有机酸类等化学成分，并对其药材来源进行了归属。结论 利用UHPLC-Q-Orbitrap HRMS建立的鉴别方法，能够准确、系统、快速地鉴定丹灯通脑胶囊中的多种化学成分，为研究丹灯通脑胶囊药效物质基础及其质量标准提供依据和参考。

Abstract:

OBJECTIVE To identify the chemical constituents in Dandeng Tongnao capsule by ultra high performance liquid chromatography-Q exactive hybrid quadrupole-orbitrap high-resolution accurate mass spectrometry(UHPLC-Q-Orbitrap HRMS). METHODS The ACQUITY UPLC^® BEH C₁₈ chromatographic column(2.1 mm×50 mm, 1.7 μm) was used for UPLC, and the acetonitrile-0.1% formic acid water was used as mobile phase to separate various chemical constituents by gradient elution separation. Chromatographic effluent was detected by UHPLC-Q-Orbitrap HRMS full scan in positive and negative ion mode. According to precise molecular weight of compounds and multistage fragment ion information detected by UHPLC-Q-Orbitrap HRMS, reference and database information, it could be analyzed accurate characterization of the compound compared with relative retention time and mass spectrometry data of control sample. RESULTS Fifty-nine chemical constituents which mainly including flavonoids, quinones, and organic acids were identified and classified. CONCLUSION A variety of chemical constituents can be accurately identified by UHPLC-Q-Orbitrap HRMS. The results can be consulted by the further study of the pharmacodynamic basis and quality standard of Dandeng Tongnao capsule.