基于UPLC-Q-TOF MS的吴茱萸致肝毒性部位及入血成分分析
Analysis of Euodia rutaecarpa Hepatotoxic Part and Absorbed Components in Rat Serum Based on UPLC-Q-TOF MS
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摘要: 利用超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF MS）法分析鉴定吴茱萸肝毒性部位的化学成分和给大鼠灌胃毒性部位后的血中原形成分及代谢产物。在优化的色谱和质谱条件下，采用正离子扫描模式对质量范围m/z 50~1 200的化合物进行数据采集，分析时间仅为12 min。通过UNIFI软件与人工相结合的方式对采集的数据进行分析，根据高分辨质谱提供的母离子与碎片离子的精确质量信息，初步推测了化合物的分子组成；结合标准品和参考文献数据，共鉴定了肝毒性部位中的29个化学成分，其中包括9个吲哚类生物碱、10个喹诺酮类生物碱、5个三萜、3个黄酮、1个其他类生物碱和1个有机酸。进一步比较了体内外样品的基峰离子色谱图，结合质谱数据和化合物裂解规律，共鉴定出21个入血成分，包括15个原形成分和6个代谢产物（1个为未知成分），并推测了代谢产物的代谢途径。该方法可为揭示吴茱萸肝毒性成分提供可靠的数据支持。
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关键词:
- 吴茱萸 /
- 肝毒性部位 /
- 成分分析 /
- 代谢产物 /
- 超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF MS）
Abstract: A method of ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF MS) was established to analyze the chemicals in Euodia rutaecarpa hepatotoxic part and metabolic components in rat blood. Under the optimized condition of chromatography and mass spectrometry, the data collection for the compounds in the mass range of m/z 50-1200 was performed using positive ion scanning mode within 12 min. The collected data were analyzed based on UNIFI software combined with artificial analysis. According to the precise mass information of precursor ions and fragment ions offered by high resolution mass spectrometry, the molecule composition of compound was preliminarily speculated. Finally, a total of 29 constituents in hepatotoxic part are identified combined with substances and reference data, including 9 indole alkaloids, 10 quinolone alkaloids, 5 triterpenoids, 3 flavonoids, one other alkaloid and one organic acid. 21 compounds in blood are characterized, including 15 prototypes and 6 metabolites (a compound unknown) by comparing the base peak ion chromatograms of samples in vivo and in vitro combined with MS data, compound fragmentation laws and published literatures. The metabolic pathways of metabolites were further speculated. This method can provide, a reliable data support to indicate hepatotoxic components of Euodia rutaecarpa. -
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