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基于UHPLC-Q-TOF-MS的中药吴茱萸化学成分表征与鉴定

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基于灵敏、高效的超高效液相色谱-四极杆飞行时间质谱(UHPLC-Q-TOF-MS)技术,结合自建信息数据库,系统地表征与鉴定吴茱萸的化学成分。对色谱分离条件(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、fragmentor、碰撞能量)进行优化,最终采用HSS T3 色谱柱(2。1 mm×100 mm,1。8 μm),流动相为 0。1%甲酸水-乙腈,流速 0。4 mL·min-1,柱温 35℃,电喷雾离子源,在Auto MS/MS模式下进行正、负离子模式质谱数据采集。根据对照品比对、碎片离子信息解析、相关文献及自建信息数据库检索等,从吴茱萸水煎液中共鉴定或推导了 92 个化合物,包括 33 个生物碱类、23 个黄酮类、12 个萜类、12 个苯丙素类、12 个其他类。其中 17 个化合物通过对照品比对鉴定,11 个化合物为吴茱萸中未报道成分。该研究实现了吴茱萸水煎液中多类别化学成分的快速表征与鉴定,为其药效物质与质量控制研究提供了参考。
Characterization and identification of chemical components from Euodiae Fructus based on UHPLC-Q-TOF-MS
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 mL·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,12 phenylpropanoids,and 12 others.Among them,17 compounds were identified by comparison with the reference compounds,and 11 compounds 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.

Euodiae FructusUHPLC-Q-TOF-MSchemical componentstructural characterization

王宇、胡万弟、洪莉丽、徐晓艳、王洪达、王小莹、杨文志、高秀梅

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天津中医药大学现代中药创制全国重点实验室 天津中医药大学方剂学教育部重点实验室,天津 301617

吴茱萸 UHPLC-Q-TOF-MS 化学成分 结构鉴定

国家自然科学基金重大项目国家中医药局中医药创新团队及人才支持计划

82192914ZYYCXTD-C-202009

2024

中国中药杂志
中国药学会

中国中药杂志

CSTPCD北大核心
影响因子:1.718
ISSN:1001-5302
年,卷(期):2024.49(11)