色谱 ›› 2017, Vol. 35 ›› Issue (7): 688-695.DOI: 10.3724/SP.J.1123.2017.05014

• 研究论文 • 上一篇    下一篇

聚酰基氨基脲类多孔有机聚合物的制备及其在糖肽富集中的应用

王红卫1,2, 刘忠山1, 彭孝军2, 欧俊杰1, 叶明亮1   

  1. 1. 中国科学院大连化学物理研究所, 中国科学院分离分析化学重点实验室, 辽宁 大连 116023;
    2. 大连理工大学, 精细化工国家重点实验室, 辽宁 大连 116024
  • 收稿日期:2017-05-17 出版日期:2017-07-08 发布日期:2013-10-18
  • 通讯作者: 欧俊杰,Tel:(0411)84379576,E-mail:junjieou@dicp.ac.cn;叶明亮E-mail:mingliang@dicp.ac.cn
  • 基金资助:

    国家重点研发计划(2016YFA0501402);国家自然科学基金(21575141).

Fabrication of acylsemicarbazide-based porous organic polymer for selective enrichment of glycopeptides

WANG Hongwei1,2, LIU Zhongshan1, PENG Xiaojun2, OU Junjie1, YE Mingliang1   

  1. 1. Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    2. State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, China
  • Received:2017-05-17 Online:2017-07-08 Published:2013-10-18
  • Supported by:

    China State Key Research Grant (No.2016YFA0501402);National Natural Science Foundation of China (No.21575141).

摘要:

通过均苯三甲酰肼(BTZ)和对苯二异氰酸酯(PDI)的聚合反应制备了一种新型的聚酰基氨基脲类多孔有机聚合物(POP)。采用傅里叶变换红外光谱(FT-IR)、交叉极化魔角自旋碳13核磁共振(CP-MAS 13C NMR)、氮气物理吸附/脱附实验和水接触角等手段对POP-1的物理性质进行表征。其中比表面积为166 m2/g,水接触角为46.4°,表明这种多孔材料具有良好的亲水性。因此,尝试将POP-1应用于标准蛋白质和复杂生物样品中糖肽的亲水色谱富集。通过基质辅助激光解吸电离飞行时间质谱(MALDI-TOF/MS)分析,从500 fmol人血清免疫球蛋白G(IgG)酶解液中共鉴定到19条典型的N-连接糖肽;通过毛细管液相色谱-串联质谱(cLC-MS/MS)分析,从100 μ g鼠肝蛋白酶解液中共鉴定到属于605个糖蛋白的1919个糖肽的1350个N-糖基化位点。这些结果表明POP-1在糖蛋白质组学研究中具有较强的应用潜力。

关键词: 对苯二异氰酸酯, 多孔有机聚合物, 均苯三甲酰肼, 亲水, 糖肽富集, 酰基氨基脲

Abstract:

An acylsemicarbazide-based porous organic polymer (POP) was facilely prepared by the polymerization of benzene-1,3,5-tricarbohydrazide (BTZ) and 1,4-phenylene diisocyanate (PDI). The physical properties of as-synthesized material were characterized by Fourier-transform infrared spectroscopy (FT-IR), solid-state cross polarisation magic angle spinning carbon-13 nuclear magnetic resonance (CP-MAS 13C NMR), nitrogen adsorption/desorption measurement, water contact angle and so on. The specific surface area was 166 m2/g, and the water contact angle was 46.4°, exhibiting hydrophilic property of the porous material. Thus, POP-1 was tried to be used for glycopeptides enrichment from tryptic digest of standard protein and complex biosamples in hydrophilic mode. The 19 typical N-linked glycopeptides were identified from 500 fmol tryptic digest of immunoglobulin G (IgG) from human serum by matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF/MS) analysis, meanwhile, 1919 unique glycopeptides with 1350 N-glycosylation sites from 605 different N-linked glycoproteins were identified from 100 μ g mouse liver tryptic digest by capillary liquid chromatography (cLC)-MS/MS analysis. These results demonstrated the great potential of POP-1 for glycoproteome analysis.

Key words: 1,4-phenylene diisocyanate (PDI), acylsemicarbazide, benzene-1,3,5-tricarbohydrazide (BTZ), glycopeptide enrichment, hydrophilic, porous organic polymer

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