短瓣金莲花化学成分的UPLC-Q-TOF-MS分析

Analysis on chemical constituents from flowers of Trollius ledebouri by UPLC-Q-TOF-MS

目的应用超高效液相色谱仪联用四级杆串联飞行时间质谱仪（UPLC-Q-TOF-MS）在正负离子模式下分离分析短瓣金莲花药材甲醇提取物成分。方法采用ACQUITY UPLC BEH C18色谱柱（100 mm×2.1 mm,1.7μm）,以0.1%甲酸水（A）-0.1%甲酸甲醇（B）溶液为流动相,梯度洗脱0-5 min,95%-60%A;5-13 min,60%-45%A;13-20 min,45%-0%A;20.1-25 min,95%A;体积流量0.3 m L/min,进样量2μL。通过正、负离子质谱信息及元素组成,与相关文献数据对照,分析化合物信息。结果结合UPLC-Q-TOF-MS提供的化合物准确相对分子质量,鉴定短瓣金莲花提取物中14个化合物,分别为藜芦酸、香草酸、荭草苷、荭草素-2″-O-β-L-半乳糖苷、荭草苷-2″-O-β-D-吡喃木糖苷、槲皮素、金丝桃苷、牡荆苷、芹菜素、木犀草素、刺槐素-7-O-新橙皮糖苷、刺槐素、柳穿鱼黄素、鼠尾草素。结论该法为短瓣金莲花饮片的质量控制、后期临床应用提供技术支持,并为阐明其药效物质基础提供参考。

Objective The chemical constituents in the methanol extract from the flowers of Trollius ledebouri were rapidly identified using UPLC-Q-TOF-MS in positive and negative ion modes. Methods The analysis was performed on an ACQUITY UPLC BEH C18 reverse phase column（100 mm × 2.1 mm, 1.7 μm）. The mobile phase consisted of methanol and 0.1% formic acid was used for gradient elution, 0—5 min, 95%—60% A; 5—13 min, 60%—45% A; 13—20 min, 45%—0% A; 20.1—25 min, 95% A. The flow rate was 0.3 m L/min, the injection volume was 2 μL. The information of the compounds was analyzed by the positive and negative ion mass spectra and elements composition. Results The results indicated that 14 compounds in the extract from the flowers of T. ledebouri had been identified by direct comparison in both positive and negative ion mass data, they were vevatric acid, vanillic acid, orietin, orietin-2″-O-β-L-galactopyranoside, orietin-2″-O-β-D-xylopyranoside, quercetin, hyperoside, vitexin, apigenin, luteolin, acacetin-7-O-neohesperidoside, acacetin, pectolinarigenin, and salvigenin. Conclusion UPLC-Q-TOF-MS could be used to analyze the constituents in the extract from flowers of T. ledebouri and to provide the protection for the quality control of the pieces as well as the stability and efficacy in the late stage clinical application, and to provide a reference for clarifying the material basis of its efficacy.