基于UPLC-Q-TOF-MS技术的当药化学成分分析

Analysis of Chemical Constituents in Swertiae Herba by UPLC-Q-TOF-MS

目的:采用超高效液相色谱-四级杆-飞行时间质谱法(UPLC-Q-TOF-MS)分析当药中主要成分。方法:采用LC-TripleTOF■5600+进行分析,色谱柱为KinetexXB-C_(18)(100 mm×2.1 mm,2.6μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,流速为0.3 mL·min^(−1),柱温20℃,质谱定性鉴别采用正离子和负离子扫描模式,扫描质量数为m/z 100~1000。使用PeakView 2.0质谱图分析软件对所得到的母离子、同位素离子及碎片离子进行分析。结果:通过对照品指认、软件预测分析并结合文献报道,共鉴定出当药中29个化合物,包括7个环烯醚萜类、13个[口山]酮类、4个黄酮类、2个三萜类、2个生物碱类和1个核苷类成分。其中10个成分为首次在当药中报道。结论:所建立的UPLC-Q-TOF-MS可为鉴定当药中的化学成分提供一种快速、高效的方法;对当药中的主要成分进行了整理,为其药效物质基础研究、多元质量评价方法的建立提供参考。

Objective:To analyze the main chemical constituents in Swertiae Herba by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS).Methods:The analysis was performed on a LC-TripleTOF■5600+system under the following conditions:chromatographic column:Kinetex XB-C_(18) column(100 mm×2.1 mm,2.6μm);mobile phase:acetonitrile-0.1%formic acid in water;gradient elution;flow rate:0.3 mL·min^(−1);column temperature:20℃.Following mass spectrometry in both the positive and negative ESI modes for qualitative identification,with the scanning range of m/z 100-1000,the resulting parent,isotopic,and fragment ions were analyzed by PeakView 2.0.Results:A total of 29 components were identified in Swertiae Herba based on reference substance identification,software prediction,and related literature reports,including 7 iridoids,13 xanthonoids,4 flavonoids,2 triterpenoids,2 alkaloids,and 1 nucleoside.Ten of them were reported for the first time.Conclusion:The established UPLC-Q-TOF-MS is a rapid and efficient method for identifying the chemical constituents in Swertiae Herba,which provides reference for the research on its pharmacodynamic substance basis and the establishment of multiple quality assessment methods.