基于UFLC-Q-TOF/MS技术的八月札化学成分研究

Chemical constituents in Akebiae Fructus based on UFLC-Q-TOF/MS

目的采用快速液相与四极杆飞行时间串联质谱(UFLC-Q-TOF/MS)联用技术分析鉴定八月札Akebiae Fructus的化学成分。方法采用Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%甲酸-乙腈和0.1%甲酸-水为流动相进行快速梯度洗脱,体积流量0.3 mL/min,柱温40℃,进样量1μL。质谱定性采用电喷雾离子源(ESI)的飞行时间质谱,负离子模式下采集数据,全扫描的质量扫描范围m/z 100～1 500。结果依据质谱裂解规律,从八月札的甲醇提取物中共鉴定出25个三萜类成分,并对另外9个未知成分进行了结构推测。结论 UFLC-Q-TOF/MS方法能够快速、准确、全面地鉴定八月札中的多种成分,为八月札的进一步提取分离和药理作用机制研究提供依据。

Objective To identify the chemical constituents in Akebiae Fructus by UFLC-Q-TOF/MS method. Methods The separation was performed on an Acquity UPLC B EH CI8 Column （100 mm× 2.1 mm, 1.7 μm）, with a mobile phase using 0.1% formic acid-acetorfitrile and water containing 0.1% formic acid （B） for gradient elution. The flow rate was 0.3 mL/min, the temperature of column was 40 ℃ with injection volume of 1μL. TOF/MS and electrospray ion （ESI） source were applied for the qualitative analysis under the negative ion mode, and the full mass scan range was m/z 100---1 500. Results According to MS principle, twenty-five triterpenoids were identified from the methanol extract of Akebiae Fructus and the chemical structures of other nine unknown compounds were deduced. Conclusion UFLC-Q-TOF/MS method could identify the main chemical constituents in Akebiae Fructus rapidly and accurately, which lays a foundation for the quality control ofAkebiae Fructus.