基于UPLC-Q-TOF-MS/MS的皖贝母生物碱类化学成分分析

Analysis of Alkaloids from Bulbs of Fritillaria anhuiensis Based on UPLC-Q-TOF-MS/MS

目的:采用超高效液相色谱串联四级杆飞行时间质谱法(UPLC-Q-TOF-MS/MS)对皖贝母醇提取物的生物碱类化学成分进行分析鉴定。方法:采用CORTECSC18色谱柱(150 mm×4.6 mm,2.7μm),流动相为乙腈-0.1%甲酸和10 mmol·L^(-1)甲酸铵水溶液,梯度洗脱,流速为0.40 mL·min^(-1),进样体积为2μL。质谱使用电喷雾离子源(ESI),正离子模式扫描采集数据。结果:通过二级高分辨质谱分析结合对照品数据及相关文献,共鉴定出皖贝母醇提取物中14个化合物的结构,包括生物碱类成分12个、非生物碱类2个,其中8个成分为首次从皖贝母中鉴定出来。结论:采用UPLC-Q-TOF-MS/MS建立了快速分析皖贝母中生物碱类化学成分的方法,该法快速、准确,为皖贝母生物碱化学成分鉴定提供了新的策略,并为皖贝母质量控制和物质基础研究提供了参考。

Objective:To analyze and identify the alkaloid components from the alcoholic extract of bulbs of Fritillaria anhuiensis by ultra performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS).Methods:The chromatographic separation was conducted on a CORTECS C18 column(150 mm×4.6 mm,2.7μm)with gradient elution of acetonitrile-0.1%formic acid and 10 mmol·L^(-1) ammonium formate solution as mobile phases at a flow rate of 0.40 mL·min^(-1)and an injection volume of 2μL.The mass spectrometry was performed using an electrospray ionization(ESI)source with positive ion mode scan for data acquisition.Results:By combining the secondary high-resolution mass spectrometry with the control data and related literature,we identified the structures of 14 compounds,including 12 alkaloids and 2 non-alkaloids,among which 8 components were identified for the first time from bulbs of F.anhuiensis.Conclusion:The method is rapid and accurate,which provides a new strategy for the identification of alkaloid components from bulbs of F.anhuiensis,and provides technical support for their further quality control and material basis research.