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基于超高效液相色谱-四极杆飞行时间质谱联用技术对吴茱萸果实化学成分的表征与鉴定

[Characterization and identification of chemical components from Euodiae Fructus based on UHPLC-Q-TOF-MS].

作者信息

Wang Yu, Hu Wan-di, Hong Li-Li, Xu Xiao-Yan, Wang Hong-da, Wang Xiao-Ying, Yang Wen-Zhi, Gao Xiu-Mei

机构信息

National Key Laboratory of Chinese Medicine Modernization, Key Laboratory of Chinese Pharmacology of the Ministry of Education, Tianjin University of Traditional Chinese Medicine Tianjin 301617, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2024 Jun;49(11):2953-2964. doi: 10.19540/j.cnki.cjcmm.20240223.201.

Abstract

A sensitive and efficient ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry(UHPLC-Q-TOF-MS) approach was established. Based on the self-developed information library, the chemical components from Euodiae Fructus were systematically characterized and identified. The chromatographic separation conditions(e. g., stationary phase,mobile phase, column temperature, and elution gradient) and MS detection conditions(nozzle voltage, capillary voltage, fragmentor,and collision energy) were optimized. Ultimately, an HSS T3 column(2. 1 mm×100 mm, 1. 8 μm) maintained at 35 ℃ was used,and 0. 1% formic acid water-acetonitrile at the flow rate of 0. 4 m L·min~(-1) was used as the mobile phase. Electrospray ionization was adopted to collect the positive and negative ion mass spectrometry data in Auto MS/MS mode. According to the reference compound comparison, fragment ion information interpretation, literature, and retrieval in the self-developed information library, 92 compounds were characterized or derived from the decoction of Euodiae Fructus, including 33 alkaloids, 23 flavonoids, 12 terpenoids, 12phenylpropanoids, and 12 others. Among them, 17 compounds were identified by comparison with the reference compounds, and 11compounds were unreported from Euodiae Fructus. This study realizes the rapid characterization and identification of multi-class chemical components in the decoction of Euodiae Fructus and provides a reference for the studies regarding its effective substances and quality control.

摘要

建立了一种灵敏高效的超高效液相色谱/四极杆飞行时间质谱(UHPLC-Q-TOF-MS)方法。基于自主开发的信息库,对吴茱萸的化学成分进行了系统表征和鉴定。优化了色谱分离条件(如固定相、流动相、柱温、洗脱梯度)和质谱检测条件(喷嘴电压、毛细管电压、碎裂电压和碰撞能量)。最终,使用了一根HSS T3柱(2.1 mm×100 mm,1.8 μm),柱温保持在35℃,以0.1%甲酸水-乙腈为流动相,流速为0.4 mL·min⁻¹。采用电喷雾电离,以自动MS/MS模式采集正、负离子质谱数据。通过对照品比较、碎片离子信息解析、文献查阅以及在自主开发的信息库中检索,从吴茱萸汤中表征或推导得到92种化合物,包括33种生物碱、23种黄酮类化合物、12种萜类化合物、12种苯丙素类化合物以及12种其他化合物。其中,通过与对照品比较鉴定出17种化合物,有11种化合物在吴茱萸中未见报道。本研究实现了吴茱萸汤中多类化学成分的快速表征和鉴定,为其有效物质及质量控制研究提供了参考。

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