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化学学报
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化学学报 ›› 2007, Vol. 65 ›› Issue (23): 2761-2764. 上一篇    下一篇

研究论文

1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生化寡糖链的HPLC分离及其激光解吸电离质谱分析

王仲孚, 张英, 林雪, 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省部共建教育部重点实验室
    陕西省生物技术重点实验室 西安 710069)
  • 投稿日期:2007-04-19 修回日期:2007-06-22 发布日期:2007-12-14
  • 通讯作者: 黄琳娟

HPLC Separation of 1-Phenyl-3-methyl-5-pyrazolone Derivatized Oligosaccharides and Its Matrix-assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry Identification

WANG Zhong-Fu; ZHANG Ying; LIN Xue; HUANG Lin-Juan*   

  1. (Key Laboratory of Resource Biology and Biotechnology in Western China, Ministry of Education, Shaanxi Provincial Key Laboratory of Biotechnology, Life Science College, Northwest University, Xi'an 710069)
  • Received:2007-04-19 Revised:2007-06-22 Published:2007-12-14
  • Contact: HUANG Lin-Juan

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2163

被引次数

78

以1-苯基-3-甲基-5-吡唑啉酮(PMP)为衍生化试剂对寡糖链进行标记, 用氨水替代氢氧化钠溶液作碱性介质, 衍生化反应后氨水可通过干燥除去, 省去了脱盐处理过程, 衍生化的寡糖可直接进行激光解吸电离质谱分析. 建立起了PMP衍生化寡糖的RP-HPLC分离分析模式, 在此HPLC分析条件下, 可以对标记的寡糖链进行样品分离及制备.

关键词: 高效液相色谱, 基质辅助激光解吸电离质谱, 1-苯基-3-甲基-5-吡唑啉酮, 衍生化, 寡糖

A modified 1-phenyl-3-methyl-5-pyrazolone (PMP) pre-column derivatization procedure has been applied to oligosaccharide separation and analysis by reversed-phase high performance liquid chromatography (RP-HPLC) and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). The traditional derivatization procedure of oligosaccharides with PMP has been simplified using liquid ammonia instead of sodium hydroxide aqueous solution as a base medium. The derivatives could be directly analyzed by MALDI-TOF-MS without a desalting procedure. The oligosaccharide-PMP derivative mixtures have been well separated and prepared by RP-HPLC under the optimized conditions using UV detection.

Key words: HPLC, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, 1-phenyl-3- methyl-5-pyrazolone, derivatization, glycan