基于UHPLC-Q-TOF-MS技术的中药补骨脂化学成分表征与鉴定

Characterization and identification of chemical components in traditionalChinese medicine Psoraleae Fructus based on UHPLC-Q-TOF-MS

建立超高效液相色谱-四极杆飞行时间质谱联用技术(UHPLC-Q-TOF-MS),结合自建化学成分数据库,系统开展中药补骨脂化学成分的表征与鉴定。通过单因素实验依次对色谱分离条件(固定相、柱温、流动相、洗脱梯度)和质谱监测的关键参数(毛细管电压、喷嘴电压、Fragmentor)进行了优化,最终采用BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸水-乙腈,流速0.4 mL·min^(-1),柱温30℃,在正、负离子模式下采用Auto MS/MS进行数据采集。通过对照品比对、二级质谱裂解碎片解析、自建数据库检索以及文献分析等,从中药补骨脂中共鉴定或初步推导了83种化合物,包括58种黄酮类、11种香豆素类、4种萜酚类、10种其他类。其中有16种化合物通过与对照品比对获得鉴定,10种化合物可能尚未从补骨脂中报道。该研究对补骨脂中的化学成分进行快速定性分析,为阐释其物质基础、促进质量控制提供了有益参考。

This study was designed to comprehensively characterize and identify the chemical components in traditional Chinese medicine Psoraleae Fructus by establishing an ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF-MS)method in combination with in-house library.The chromatographic separation conditions(stationary phase,column temperature,mobile phase,and elution gradient)and key MS monitoring parameters(capillary voltage,nozzle voltage,and fragmentor)were sequentially optimized via single-factor experiments.A BEH C_(18 )column(2.1 mm×100 mm,1.7μm)was finally adopted,with the mobile phase consisting of 0.1%formic acid in water(A)and acetonitrile(B)at the flow rate of 0.4 mL·min^(-1) and column temperature of 30℃.Auto MS/MS was utilized for data acquisition in both positive and negative ion modes.By comparison with reference compounds,analysis of the MS2 fragments,in-house library retrieval and literature research,83 compounds were identified or tentatively characterized from Psoraleae Fructus,including 58 flavonoids,11 coumarins,4 terpenoid phenols,and 10 others.Sixteen of them were identified by comparison with reference compounds,and ten compounds may have not been reported from Psoraleae Fructus.This study achieved a rapid qualitative analysis on the chemical components in Psoraleae Fructus,which provided useful reference for elucidating its material basis and promoting the quality control.