基于RRLC-DAD-ESI-Q-TOF-MS技术的山东金银花多指标定量指纹图谱分析

目的:运用RRLC-DAD-ESI-Q-TOF-MS技术分析和测定金银花中主要化学成分,建立山东金银花多指标定量指纹图谱。方法:采用RRLC-DAD-ESI-Q-TOF-MS技术对金银花提取物进行快速分析,根据获得的精确相对分子质量和二级质谱碎片信息推断化合物分子式,结合数据库和文献对金银花中化学成分进行鉴别,采用RRLC-DAD法分析测定山东金银花、河南金银花和湖南山银花中主要化学成分含量,在此基础上建立了山东金银花多指标定量指纹图谱。结果:从山东金银花中检测到51种化学成分,鉴定了其中32种化学成分;对比测定了山东金银花、河南金银花和湖南山银花中10种主要化学成分(马钱酸、绿原酸、咖啡酸、马钱苷、断氧化马钱苷、芦丁、金桃苷、木犀草苷、异绿原酸A和异绿原酸C)的含量;采用指纹图谱结合相似度分析可以实现不同品种金银花和湖南山银花的正确区分,所得结果与含量测定结果一致。结论:RRLC-DAD-ESIQ-TOF-MS技术分析速度快、灵敏度高、能够提供化合物及其碎片离子的精确质量信息,可以快速准确地鉴别和测定金银花中的化学成分。在此基础上建立的山东道地金银花的多指标定量指纹图谱,为山东金银花质量评价研究提供了技术支持。

Multiple Indicator Quantitative Fingerprint of Lonicerae Japonicae Flos from Shandong Province Based on RRLC-DAD-ESI-Q-TOF-MS

Objective: To identify and determine the main chemical constituents in Lonicerae Japonicae Flos by RRLC-DAD-ESI-Q-TOF-MS, and establish the quantitative fingerprint of Lonicerae Japonicae Flos of Shandong province. Method: The rapid analysis of Lonicerae Japonicae Flos extract was carried out by RRLC-DAD-ESI-Q-TOF-MS. The chemical formula of Lonicerae Japonicae Flos was inferred by using the exact molecular weight and secondary mass spectrometry information. The chemical compositions of Lonicerae japonicae flos were identified by data base combined with literature reviewing. The contents of main chemical components in Lonicerae Japonicae Flos from Shandong and Henan as well as Lonicerae Flos were determined by using RRLC-DAD method, and the quantitative fingerprint was established on this basis for the quality evaluation of different samples. Result: The 51 chromatographic peaks were detected and 32 chemical constituents were identified from Lonicerae Japonicae Flos. The contents of 10 major chemical contents (loganic acid,chlorogenic acid, caffeic acid, loganin,secoxyloganin, rutin,hyperoside,luteoloside,isochlorogenic acid A and isochlorogenic acid C) in Lonicerae Japonicae Flos from Shandong and Henan as well as Lonicerae Flos were determined and compared. The differentiation of different species of Lonicerae Japonicae Flos and Lonicerae Flos was achieved by RRLC fingerprint combined with similarity analysis, and the result wasconsistent with the content determination result. Conclusion: RRLC-DAD-ESI-Q-TOF-MS technique is fast and accurate, providing accurate quality information for compounds and their fragment ions. It can quickly and accurately identify and determine the chemical compositions of Lonicerae Japonicae Flos, and the multiple indicator quantitative fingerprint based on this study could provide technology support for the quality evaluation of Lonicerae Japonicae Flos.