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化学学报
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化学学报 ›› 2011, Vol. 69 ›› Issue (14): 1697-1704. 上一篇    下一篇

研究论文

κ-卡拉胶寡糖AEC柱前衍生物的LC-ESI-MS/MSn分离分析

孙玉姣，王承建，耿腾飞，王仲孚，黄琳娟*   

  1. (西北大学生命科学学院 西部资源生物与现代生物技术教育部重点实验室 西安 710069)
  • 投稿日期:2010-12-01 修回日期:2011-05-18 发布日期:2011-06-19
  • 通讯作者: 王珍 E-mail:wangzh@163.com
  • 基金资助:

    国家自然科学基金;教育部新世纪优秀人才支持计划;陕西省重点实验室重点科研计划项目

Analysis of κ-Carrageenan Oligosaccharides by LC-ESI-MS/MSn with 3-Amino-9-ethylcarbazole Derivatization

SUN Yu-Jiao, WANG Cheng-Jian, GENG Teng-Fei, WANG Zhong-Fu, HUANG Lin-Juan   

  1. (Key Laboratory of Ministry of Education for Western China Resource Biology and Biotechnology, Life Science College, Northwest University, Xian 710069)
  • Received:2010-12-01 Revised:2011-05-18 Published:2011-06-19

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以κ-卡拉胶为原料, 经盐酸水解得到一系列寡糖混合物. 以3-氨基-9-乙基咔唑(3-amino-9-ethylcarbazole, AEC)为衍生化试剂, 对酸解得到的κ-卡拉胶寡糖进行柱前衍生, 采用反相C18色谱柱(250 mm×4.6 mm, 5 μm), 乙腈和乙酸铵水溶液(pH 4.5)为流动相, 梯度洗脱, 在254 nm波长处检测, 建立了κ-卡拉胶寡糖衍生物的高效液相色谱(HPLC)分离以及液相色谱-电喷雾质谱联用(LC-ESI-MS)分离分析的方法, 并对AEC衍生后的κ-卡拉胶寡糖进行多级质谱裂解(MSn), 进一步获得了κ-卡拉胶寡糖的结构信息. 该方法对κ-卡拉胶寡糖的结构分析、构效关系等方面的研究有参考价值.

关键词: κ-卡拉胶寡糖, 3-氨基-9-乙基咔唑, 液相色谱-电喷雾质谱联用, 多级质谱裂解

A series of κ-carrageenan oligosaccharides were prepared by using hydrochloric acid hydrolysis. The κ-carrageenan oligosaccharides derivatized with 3-amino-9-ethylcarbazole (AEC) were analyzed by high performance liquid chromatography (HPLC) and HPLC coupling with electrospray ionization ion-trap mass spectrometry (LC-ESI-MS). The HPLC separation was carried out on a reverse phase (RP) C18 column (250 mm×4.6 mm, 5 μm) in a linear gradient mode, using acetonitrile and ammonium acetate aqueous solution (pH 4.5) as mobile phase and a ultraviolet (UV) detection at 254 nm. Furthermore, the structure of the κ-carrageenan oligosaccharide was confirmed by multi-stage mass spectrometry (MSn). These results may be helpful to investigation in structure identification and structure-activity relationship of κ-carrageenan oligosaccharides.

Key words: κ-carrageenan oligosaccharides, 3-amino-9-ethylcarbazole, high performance liquid chromato- graphy coupling with electrospray ionization ion-trap mass spectrometry (LC-ESI-MS), mass spectrometry (MSn)

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