摘要
采用超高效液相色谱-四级杆静电轨道阱质谱联用技术,对柴胡的化学成分进行快速鉴定。使用ACQUITY UPLCHSS T3(100 mm×2.1 mm,1.8μm)色谱柱,以0.05%甲酸水溶液-0.05%甲酸乙腈溶液为流动相进行梯度洗脱,在电喷雾离子源(ESI)正负离子监测模式下对样品进行数据采集。利用高分辨质谱数据,结合文献、对照品质谱数据、Mass Frontier验证,从柴胡中鉴定出65种成分,包括32种皂苷类成分,11种黄酮类成分,18种酸类成分,4种其它成分,其中壬二酸、3,5,6-三羟基-4’,7-二甲氧基黄酮、13-羟基-9,11-十八二烯酸、甲氧基-十五烷酸4种成分为首次在柴胡中发现。该方法可为柴胡的快速鉴定、药效基础发现和质量控制方法建立提供参考。
A method of ultra-performance liquid chromatography coupled with hybrid quadrupole-orbitrap mass spectrometry(UPLC-Q-Exactive Orbitrap MS)was developed to rapidly identification of the chemical constituents in Bupleuri Radix.Waters ACQUITY UPLCHSS T3 column(100 mm×2.1 mm,1.8μm)was used as the separation column,the mobile phase was 0.05%formic acid in water and 0.05%formic acid in acetonitrile.Mass spectrometric analysis was performed in the positive and negative electrospray ionization(ESI)modes.Based on high resolution mass spectrometry data,references,standard mass spectrometry data and Mass Frontier validation,65 compounds were identified in Bupleuri Radix,including 32 saponins,11 flavonoids,18 acids and 4 other components.Among them,azelaic acid,3,5,6-Trihydroxy-4’,7-dimethoxyflavone,13-hydroxy-9,11-octadecadienoic acid,methoxy-pentadecanoic acid were discovered in Bupleuri Radix for the first time.This method can provide reference for the rapid identification of Bupleuri Radix,the discovery of efficacy basis and the establishment of quality control methods.
作者
刘月程
田振华
LIU Yuecheng;TIAN Zhenhua(Shandong Academy of Chinese Medicine,Jinan 250014,China;Experimental Center,Shandong University of Traditional Chinese Medicine,Jinan 250355,China)
出处
《化学分析计量》
CAS
2022年第8期5-12,共8页
Chemical Analysis And Meterage
基金
山东省医药卫生科技发展计划项目(202113030924)。