基于UPLC-Q-TOF/MS技术分析加味左金丸化学成分及指纹图谱研究

Chemical components and chromatographic fingerprints of Jiawei Zuojin Pill based on UPLC-Q-TOF/MS

目的 采用UPLC-Q-TOF/MS技术对加味左金丸中的化学成分进行定性分析。方法 色谱柱为ACQUITY Premier BEH C_(18)(100 mm×2.1 mm,1.8μm),流动相为乙睛-甲醇-0.1%甲酸水溶液,梯度洗脱,体积流量为0.3 mL/min;质谱的离子源为ESI,模式为正、负离子模式。通过质谱给出的分子离子峰和二级质谱碎片离子峰,结合对照品的相对保留时间,参考相关的文献,对于加味左金丸中的化学成分进行鉴定。并建立不同批次加味左金丸样品的指纹图谱。结果 通过对数据的分析,从加味左金丸中鉴定出92个成分,其中包括16个有机酸类成分、34个黄酮类成分、17个生物碱类成分、21个萜类成分与4个其他类成分。建立的加味左金丸指纹图谱有13个共有峰,分别为黄芩苷、山柰酚-3-O-葡萄糖苷、槲皮素、汉黄芩素、甘草素、千层纸素A、芍药苷、吴茱萸次碱、小檗碱、巴马汀、枸橘苷、橙皮苷、柴胡皂苷d。指纹图谱方法的精密度、稳定性、重复性良好,多批次加味左金丸的成分基本一致。结论 建立的UPLC-Q-TOF/MS方法对化学成分进行了鉴定,建立的指纹图谱方法为进一步分析加味左金丸的物质基础提供了重要依据。

Objective To qualitatively analyze the main chemical constituents of traditional Chinese medicine compound Jiawei Zuojin Pill(加味左金丸) by using UPLC-Q-TOF/MS technology.Methods The separation was performed on ACQUITY Premier BEH C_(18) column(100 mm×2.1 mm,1.8 μm),and the gradient elution of acetonitrile-methanol-0.1% formic acid was used as mobile phase at a flow rate of 0.3 mL/min.The data was collected by the positive and negative ion modes using Q-TOF/MS and ESI source.The main chemical constituents of Jiawei Zuojin Pill were identified according to the exact molecular mass,the cleavage fragments of MS/MS,the literature data,and the reference control.And chromatographic fingerprints of different batches of Jiawei Zuojin Pill were established.Results A total of 92 chemical components were identified in Jiawei Zuojin Pill,including 16 organic acids,34 flavonoids,17 alkaloids,21 terpenoid and four other components.The HPLC fingerprint of Jiawei Zuojin Pill was established with 13 common peaks,which were baicalin,astragalin,quercetin,wogonin,liquiritigenin,oroxylin A,paeoniflorin,rutecarpine,berberine,palmatine,poncirin,hesperidin,saikosaponin d.And the precision,stability and reproducibility of the HPLC fingerprint were acceptable.The components in different batches of Jiawei Zuojin Pill were basically similar.Conclusion This study showed that UPLC-Q-TOF/MS technology provided a rapid and accurate method for the identification of chemical constituents in Jiawei Zuojin Pill.The HPLC fingerprint could provide an important basis for the quality control and pharmacodynamic material basis study of Jiawei Zuojin Pill.