色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 876-882.DOI: 10.3724/SP.J.1123.2012.05021

• 研究论文 • 上一篇    下一篇

银离子高效液相色谱-质谱法分析血清中甘油三酯类化合物的组成

杨芹, 石先哲*, 单圆鸿, 窦阿波, 许国旺   

  1. 中国科学院大连化学物理研究所, 中国科学院分离分析重点实验室, 辽宁 大连 116023
  • 收稿日期:2012-05-11 修回日期:2012-06-04 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 石先哲,博士,副研究员,主要从事色谱-质谱联用及代谢组学研究. E-mail: shixianzhe@dicp.ac.cn.
  • 基金资助:

    国家自然科学基金项目(81060086, 20805045)和国家“973”计划课题(2012CB720801).

Triacylglyceride profiling in serum by silver ion high performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry

YANG Qin, SHI Xianzhe*, SHAN Yuanhong, DOU Abo, XU Guowang   

  1. CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China
  • Received:2012-05-11 Revised:2012-06-04 Online:2012-09-28 Published:2012-09-20

PDF

524

被引次数

17

摘要： 针对甘油三酯(TAG)类化合物的复杂性,建立了分析小鼠血清中TAG类化合物的方法。采用经典的氯仿-甲醇溶剂体系对血中的TAG类化合物进行提取。脂质提取物经Varian ChromSpher 5 Lipids柱分离,在0.75 mL/min的流速下以乙腈-正己烷(1:99, v/v)为流动相进行等度洗脱,采用大气压化学电离源正离子模式电离,质谱增强型全扫描、增强型子离子扫描和中性丢失扫描模式检测。根据银离子色谱对双键的保留规律以及质谱所给出的碎片离子信息,对血清中TAG类化合物进行了结构鉴定。结果表明采用该方法可以从小鼠血清中鉴定到66个TAG类化合物以及5个胆固醇酯。该方法简单,重现性好,可通用于其他样品中TAG类化合物的检测。

关键词: 大气压化学电离质谱, 甘油三酯类化合物, 血清, 银离子高效液相色谱

Abstract: A simple and effective method was developed to investigate triacylglyceride (TAG) compounds in biological matrices using silver ion high performance liquid chromatography-mass spectrometry (Ag+-HPLC-MS). The TAG compounds from mouse serum were extracted by a modified Folch method using the classical CHCl3-MeOH solvent system. The extract was separated on a Varian ChromSpher 5 Lipids column with isocratic elution using acetonitrile-hexane (1:99, v/v) as mobile phase at a flow rate of 0.75 mL/min, and detected by a mass spectrometer equipped with an atmospheric pressure chemical ionization (APCI) source in positive ion mode to acquire sufficient MS information of TAG compounds by enhanced mass spectrometry (EMS), enhanced product ion (EPI) and neutral loss (NL) scans. The identification of TAG compounds was based on their chromatographic behaviors and MS data. Besides, the NL scans of thirty fatty acids were performed to further validate the results. Finally, 66 TAG compounds as well as 5 cholesteryl ether (CE) compounds were obtained from the mouse serum extract. This method is simple, reproducible and also suitable for the analysis of TAG compounds in other samples.

Key words: atmospheric pressure chemical ionization mass spectrometry (APCI-MS), serum, triacylglyceride compounds, silver ion high performance liquid chromatography (Ag+-HPLC)