UPLC-Q-TOF-MSE技术结合UNIFI筛查平台分析加味逍遥丸化学成分

doi:10.19803/j.1672-8629.20211148

摘要/Abstract

摘要： 目的运用高效液相色谱-四极杆-飞行时间串联质谱法（UPLC-Q-TOF-MS^E）对加味逍遥丸的化学成分进行分析与鉴定,为复方质量控制及药效物质基础研究提供理论依据。方法采用ACQUITY UPLC BEH C₁₈柱（2.1 mm×100 mm,1.7 μm,Waters）,以0.1%甲酸水-乙腈为流动相,梯度洗脱,进样量5 μL,流速0.3 mL·min^-1,柱温40 ℃。采用电喷雾离子源,在正、负2种模式下进行复方质谱检测与分析,并且使用UNIFI平台对MS^E模式下采集的质谱数据,结合化合物准分子离子、质谱裂解途径及标准品进行结构确认。结果通过分析目标化合物的分子离子峰和二级质谱特征碎片离子,并且结合标准品裂解规律以及相关文献资料,共鉴定了其中78个化学成分,包括3个倍半萜类成分、4个苯丙素类成分、13个单萜类成分、7个酚类成分、5个环烯醚萜类成分、10个黄酮类成分、23个三萜类成分及13个其他类成分。结论运用UPLC-Q-TOF-MS^E技术可快速分析鉴定复方加味逍遥丸的主要化合物类型,可为复方质量控制及药效物质基础研究提供理论依据。

关键词: 加味逍遥丸, 高效液相色谱-四级杆-飞行时间串联质谱法（UPLC-Q-TOF-MS^E）, 化学成分, UNIFI平台

Abstract: Objective To analyze and identify the chemical constituents of Jiawei Xiaoyao pills with high performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS^E) so as to provide data for quality control of the compound. Methods The ACQUITY UPLC BEH C18 column (2.1×100 mm, 1.7 μm, Waters) was used with 0.1% formic acid water-acetonitrile as the mobile phase. The injection volume was 5 μL, the flow rate 0.3 mL·min^-1, and the column temperature 40℃. Electrospray ionization (ESI) ion source was used for compound mass spectrometry detection and analysis in positive and negative modes. Structural confirmation was accomplished based on data on mass spectrometry collected from the UNIFI platform in the MS^E mode in combination with compound excimer ions, mass spectrum cleavage pathway and reference substance. Results A total of 78 chemical components were identified by analyzing the molecular ion peaks and secondary mass spectrometry characteristic fragment ions of the target compound, and according to the cracking of reference substances and related literature. There were 3 sesquiterpenoids, 4 phenylpropanoids, 13 monoterpenoids, 7 phenols, 5 iridoids, 10 flavonoids, 23 triterpenoids and 13 other compounds. Conclusion UPLC-Q-TOF-MS^E technology can be used to quickly analyze and identify the main compound types of compound Jiawei Xiaoyao pills, which can provide data for quality control of the compound and for subsequent studies on the substance basis of pharmacodynamics.

Key words: Jiawei Xiaoyao pill, UPLC-Q-TOF-MS^E, chemical composition, UNIFI platform

中图分类号:

R927

孙健, 刘子维, 刘莹, 张美玉, 李孟莹, 张海鸣, 聂颖兰, 权建野, 闫寒, 彭娟, 栗俞程, 杨书彬. UPLC-Q-TOF-MS^E技术结合UNIFI筛查平台分析加味逍遥丸化学成分[J]. 中国药物警戒, 2023, 20(2): 181-190.

SUN Jian, LIU Ziwei, LIU Ying, ZHANG Meiyu, LI Mengying, ZHANG Haiming, NIE Yinglan, QUAN Jianye, YAN Han, PENG Juan, LI Yucheng, YANG Shubin. Identification of chemical constituents in Jiawei Xiaoyao pills by UPLC-Q-TOF-MS^Ecombined with UNIFI informatics platform[J]. Chinese Journal of Pharmacovigilance, 2023, 20(2): 181-190.

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