经典名方达原饮化学成分的UPLC-Q-Exactive Orbitrap MS快速表征

Rapid Characterization of Chemical Constituents in Dayuanyin by UPLC-Q-Exactive Orbitrap MS

目的:基于超高效液相色谱-四极杆/静电场轨道阱质谱法(UPLC-Q-Exactive Orbitrap MS)对达原饮的化学成分进行定性分析。方法:采用Thermo Acclaim^(TM)RSLC 120 C_(18)色谱柱(2.1 mm×100 mm,2.2μm),流动相选择乙腈(A)-0.1%甲酸水溶液(B)梯度洗脱(0~7.5 min,10%~19%A;7.5~12 min,19%~22.5%A;12~23 min,22.5%~27%A;23~27 min,27%~56%A;27~35 min,56%~84%A;35~36 min,84%~90%A),流速0.3 mL·min^(-1),柱温30℃,加热电喷雾离子源(HESI),正、负离子模式下采集数据,检测范围m/z 80~1200。结合对照品保留时间、碎片离子、Pub Chem等数据库及相关文献信息,运用Xcalibur 3.0完成对达原饮中化学成分的定性鉴别。结果:从达原饮中共表征出161个化学成分,包括生物碱类14个、黄酮类60个、萜类16个、皂苷类26个、苯丙素类18个、有机酸16个、其他类11个。结论:建立的UPLC-Q-Exactive Orbitrap MS能有效、快速识别达原饮中化学成分,明确其化学组成,可为该经典名方的中药复方制剂开发提供依据。

Objective:To characterize the chemical constituents of Dayuanyin based on ultra-performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry(UPLC-Q-Exactive Orbitrap MS).Method:The detection was performed on a Thermo Acclaim^(TM)RSLC 120 C_(18) column(2.1 mm×100 mm,2.2μm),the mobile phase was acetonitrile(A)-0.1%formic acid aqueous solution(B)for gradient elution(0-7.5 min,10%-19%A;7.5-12 min,19%-22.5%A;12-23 min,22.5%-27%A;23-27 min,27%-56%A;27-35 min,56%-84%A;35-36 min,84%-90%A),the flow rate was 0.3 mL·min-1,and the column temperature was 30℃.The data were collected in the positive and negative ion modes by heated electrospray ionization(HESI),and the detection range was m/z 80-1200.Combining the retention time of the reference substance,fragment ions,databases such as PubChem and related literature,Xcalibur 3.0 was used to identify the chemical constituents of Dayuanyin.Result:A total of 161 compounds were identified,including 14 alkaloids,60 flavonoids,16 terpenoids,26 saponins,18 phenylpropanoids,16 organic acids and 11 others.Conclusion:The established method can effectively and quickly identify the chemical components in Dayuanyin,and clarify its chemical composition,which can provide a basis for the development of compound preparations of this famous classical formula.