基于UPLC-Q-Exactive Focus-MS/MS技术分析飞蛾藤中的化学成分

Chemical constituents in Porana racemosa Roxb.by UPLC-Q-Exactive Focus-MS/MS

目的使用超高效液相色谱-四极杆-静电场轨道离子阱联用质谱(UPLC-Q-Exactive Focus-MS/MS)技术对飞蛾藤中化学成分进行快速解析。方法80%甲醇超声提取飞蛾藤药材作为供试品,采用Thermo Accucore aQ C_(18)色谱柱(2.1 mm×150 mm,2.6μm),流动相甲醇(A)-0.1%甲酸水溶液(B),梯度洗脱(0~12 min,5%~25%A;12~20 min,25%~30%A;20~28 min,30%~38%A;28~40 min,38%~50%A;40~55 min,50%~60%A);流速0.3 mL·min^(-1),柱温30℃,进样量3μL;采用高性能加热电喷雾离子源(HESI),正、负离子监测模式,扫描范围m/z 80~1200。结果从飞蛾藤中共鉴定出30个化学成分,包括有机酸类13个、香豆素类5个、酰胺类4个、黄酮类3个及其他类5个,其中9个成分经与对照品比对后准确鉴定,7个成分在飞蛾藤属植物中首次发现。结论本方法能够对飞蛾藤中的化学成分进行快速、全面地分析,可为飞蛾藤的药效物质及质量控制研究提供依据。

Objective To rapidly recognize and identify the chemical compounds in Porana racemosa by ultra-high performance liquid chromatography coupled with Q-Exactive Focus mass spectrometry(UPLC-Q-Exactive Focus-MS/MS).Methods Methanol extract(80%)was used as the test sample to identify the chemical compounds of Porana racemosa.Thermo Accucore aQ C_(18) column(2.1 mm×150 mm,2.6μm)was used for the separation.The mobile phase consisted of methanol(A)-0.1%formic acid solution(B),gradient elution(0~12 min,5%~25%A;12~20 min,25%~30%A;20~28 min,30%~38%A;28~40 min,38%~50%A;40~55 min,50%~60%A).The flow rate was 0.3 mL·min^(-1),the column temperature was 30℃,and the injection volume was 3μL.Data were collected in both positive and negative modes.The scanning range was m/z 80~1200.Results Totally 30 chemical constituents from Porana racemosa were identified,including 13 organic acids,5 coumarins,4 amides,3 flavonoids,and 5 others.Among them,9 compounds were unambiguously identified by comparing with reference standards,and 7 were reported for the first time in Porana plants.Conclusion This method can be used to analyze chemical compositions quickly and comprehensively in Porana racemosa.This paper provides a reference for further study on pharmacodynamic materials and quality assessment of Porana racemosa.