基于HPLC-LTQ-Orbitrap MS/MS技术的复方鱼腥草合剂化学物质基础表征研究

Analysis of Chemical Material Basis of Compound Yuxingcao Mixture Based on HPLC-LTQ-Orbitrap MS/MS Technology

目的:全面表征并归属复方鱼腥草合剂的化学物质基础。方法:采用HPLC-LTQ-Orbitrap-MS/MS快速分析方法对复方鱼腥草合剂的化学成分进行快速鉴定与归属。色谱柱为Welch Ultimate XB-C18(4.6mm×250mm,5μm),以甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,进样量为5μL,柱温为30℃,流速为1.0mL·min^-1;采用电喷雾离子源(ESI),在正、负离子模式下采集数据,离子扫描范围m/z 120~1 200。结果:通过优化液质条件后,对正负模式下的质谱信息进行分析,并结合相关文献,共鉴定出107个化学成分,其中包括11个苯乙醇苷类成分,11个环烯醚萜类成分,39个黄酮类成分、12个木脂素类成分、14个有机酸类成分,另有氨基酸类、生物碱类和辅料等成分。结论:系统全面地表征了复方鱼腥草合剂中的化学物质基础及成分归属,为提升复方鱼腥草合剂质量评价体系及药效物质基础研究奠定了基础。

Objective:To comprehensively characterize and attribute the chemical material basis of Compound Yuxingcao Mixture.Methods:The chemical constituents of the Compound Yuxingcao Mixture were rapidly identified and assigned by A HPLC-LTQOrbitrap-MS/MS rapid analysis method was employed to identificate rapidly of the chemical compounds and the attribution of Compound Yuxingcao Mixture.The chromatographic separation was achieved on a Welch Ultimate XB-C18 column with methanol-water(0.1% formic acid)as mobile phase at a flow rate of 1.0 mL min^-1.The injection volume was 5μL and the column temperature was 30℃.Electrospray ionization(ESI)source was applied and operated in both positive and negative ion mode at the mass range from 120~1 200.Results:After optimizing the LC-MS conditions,the mass spectrometry information in positive and negative mode was analyzed,and total 107 components were identified and attributed.These included 11 phenylethanoid glycosides,11 iridoids,39 flavonoids,12 lignans and 14 organic acids.Amino acids,alkaloids and ingredients were also identified in the Mixture.Conclusion:This research characterized systematically and comprehensively the chemical material basis and attribution of Compound Yuxingcao Mixture,which provided an evidence for improving the quality evaluation system and pharmacodynamic substance basic research of Compound Yuxingcao Mixture.