High-performance liquid chromatography/electrospray ionization ion-trap mass spectrometry for analysis of oligosaccharides derivatized by reductive amination and N,N-dimethylation
High-performance liquid chromatography/electrospray ionization ion-trap mass spectrometry for analysis of oligosaccharides derivatized by reductive amination and N,N-dimethylation
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DOI：
10.1016/j.carres.2007.04.020
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发表时间：
2007-08-13
影响因子：
3.1
通讯作者：
Broberg, Anders
中科院分区：
文献类型：
--
作者：
Broberg, Anders
采用高效液相色谱/电喷雾离子阱质谱法（HPLC/ESI-ITMS）分析了经苄胺还原胺化和N，N-二甲基化（DMBA-寡糖）衍生的牛奶寡糖。在石墨化碳柱上用乙腈水溶液洗脱实现DMBA-低聚糖的分离，并通过正离子模式ESI-ITMS检测DMBA-低聚糖，允许样品量下降至类似于HPLC柱上注射的30 fmol单一DMBA-低聚糖。质谱仪的MS/MS操作导致诊断片段的检测，主要属于Y系列，允许异构乳低聚糖之间的区分。HPLC/ESI-ITMS/MS/MS实验表明，在分析过程中，DMBA牛奶低聚糖的岩藻糖残基迁移到修饰的还原端葡萄糖残基，这种迁移以前仅在质子加合离子中观察到。(c)2007年由Elsevier Ltd.出版
Milk oligosaccharides derivatized by reductive amination with benzylamine followed by N,N-dimethylation (DMBA-oligosaccharides), were analyzed by high-performance liquid chromatography/electro spray ionization ion-trap mass spectrometry (HPLC/ESI-ITMS). Separation of DMBA-oligosaccharides was achieved on a graphitized carbon column eluted with aqueous acetonitrile and the DMBA-oligosaccharides were detected by positive-ion mode ESI-ITMS allowing sample amounts down to similar to 30 fmol of single DMBA-oligosaccharides injected on the HPLC column. MS/MS operation of the mass spectrometer resulted in the detection of diagnostic fragments, mainly belonging to the Y-series, allowing differentiation between isomeric milk oligosaccharides. HPLC/ESI-ITMS/MS/MS experiments indicated the migration of fucose residues of the DMBA milk oligosaccharides to the modified reducing end glucose residue during analysis, a migration previously only observed for proton adduct ions. (c) 2007 Published by Elsevier Ltd.