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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
引用本文:王仲孚,张英,林雪,黄琳娟.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[J].化学学报,2007,65(23):2761-2764.
作者姓名:王仲孚  张英  林雪  黄琳娟
作者单位:(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)
基金项目:国家高技术研究发展计划(863计划) , 教育部重点科研
摘    要: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  
收稿时间:2007-04-19
修稿时间:2007-07-06

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.HPLC Separation of 1-Phenyl-3-methyl-5-pyrazolone Derivatized Oligosaccharides and Its Matrix-assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry Identification[J].Acta Chimica Sinica,2007,65(23):2761-2764.
Authors:WANG  Zhong-Fu  ZHANG  Ying  LIN  Xue  HUANG  Lin-Juan
Institution:(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)
Abstract: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.
Keywords:HPLC  matrix-assisted laser desorption/ionization time-of-flight mass spectrometry  1-phenyl-3-methyl-5-pyrazolone  derivatization  glycan
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