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-MAS13C 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 m^2/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(c LC-MS/MS)分析,从100μg鼠肝蛋白酶解液中共鉴定到属于605个糖蛋白的1 919个糖肽的1 350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。
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 13 C NMR), nitrogen adsorption desorption measurement, water contact angle and so on. The specific surface area was 166 m^2 /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, 1 919 unique glycopeptides with 1 350 N-glycosylation sites from 605 different -linked glycoproteins were identified from 100 μg mouse liver tryptic digest by capillary liquid chromatography (CLC) -MS/MS analysis. These results demonstrated the great potential of POP-1 for glycoproteome analysis.
出处
《色谱》
CAS
CSCD
北大核心
2017年第7期688-695,共8页
Chinese Journal of Chromatography
基金
国家重点研发计划(2016YFA0501402)
国家自然科学基金(21575141)~~
关键词
酰基氨基脲
多孔有机聚合物
均苯三甲酰肼
对苯二异氰酸酯
糖肽富集
亲水
acylsemicarbazide
porous organic polymer
benzene-1,3,5-tricarbohydrazide (BTZ)
1,4-phenylene diisocyanate (PDI)
glycopeptide enrichment
hydrophilic