色谱

色谱

• 研究论文 • 上一篇    下一篇

超高效液相色谱/飞行时间质谱用于人参皂甙Rg3作用后大鼠尿液代谢物指纹图谱分析及标记物的鉴定

汪江山1,赵欣捷1,郑育芳2,孔宏伟1,卢果1,蔡宗苇2, 许国旺1

  

  1. 1.National Chromatographic R. &A. Center, Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China; 2.Department of Chemistry, Hong Kong Baptist University, Hong Kong, China
  • 收稿日期:2005-08-05 修回日期:2005-10-13 出版日期:2006-01-30 发布日期:1987-09-25

Metabolite Fingerprint and Biomarkers Identification of Rat Urine after Dosed with Ginsenoside Rg3 Based on Ultra High
Performance Liquid Chromatography/Time-of-Flight Mass Spectrometry (UPLC/TOF-MS)

WANG Jiangshan1, ZHAO Xinjie1, ZHENG Yufang2, KONG Hongwei1, LU Guo1, CAI Zongwei2, XU Guowang1

  

  1. 1.National Chromatographic R. &A. Center, Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China; 2.Department of Chemistry, Hong Kong Baptist University, Hong Kong, China
  • Received:2005-08-05 Revised:2005-10-13 Online:2006-01-30 Published:1987-09-25

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摘要：

超高效液相色谱技术(UPLC)采用1.7 μm的色谱柱填料,有更好的分离效率、峰容量以及灵敏度;高分辨的时间飞行质谱(TOF-MS)能够测定化合物准确的分子质量并具有MS/MS功能。 两者的联用适合于复杂体系的分离分析和未知物的结构鉴定。 因此建立了一种基于UPLC/TOF-MS测定人参皂甙Rg3给药后大鼠尿液代谢物变化的方法,对其中2种发生显著变化的代谢物分别通过准确的质量测定得到其元素组成,通过MS/MS技术得到其结构信息,并通过检索数据库最终分别鉴定为4,8-二羟喹啉甲酸和4-羟基-2-喹啉酸。

关键词: 超高效液相色谱, 代谢物指纹图谱, 飞行时间质谱, 结构鉴定, 精确质量 , 人参, 人参皂甙

Abstract:

Porous particles of 1.7 μm was employed for ultra high performance liquid chromatography (UPLC), resulting in higher peak capacity, greater resolution and increased sensitivity in comparison with high performance liquid chromatography (HPLC). Time-of-flight mass spectrometer (TOF-MS) with a lockmass interface was used for the structure identification through exact mass and MS/MS experiment. The hyphenation of these two technologies made it a suitable platform for analysis of complex samples and identification of unknown compounds. Ginsenoside Rg3 has been considered as the major active component of Panax ginseng. Effect of the administration of a single dose of the Ginsenoside Rg3 to male Sprague Dawley rats on the urinary metabolite profiles of a range of endogenous metabolites had been investigated using UPLC/TOF-MS. Urine samples were collected from both dosed and control animals. Analysis of these samples revealed marked changes in the pattern of endogenous metabolites due to the effect of Ginsenoside Rg3. Significant disturbances in the urinary metabolite were observed in the first day after dose. Endogenous metabolites with significant up-regulation identified by accurate mass and MS/MS were xanthurenic acid, and kynurenic acid.

Key words: accurate mass , Ginsenoside, metabolite fingerprint, Panax ginseng, structure identification, time-of-flight mass spectrometry (TOF-MS), ultra high performance liquid chromatography (UPLC)