Structural characterization of pyridylaminated oligosaccharides derived from neutral glycosphingolipids by high-sensitivity capillary electrophoresis-mass spectrometry

Emi Ito, Kazuki Nakajima, Hiroaki Waki, Kozo Miseki, Takashi Shimada, Taka Aki Sato, Kazuaki Kakehi, Minoru Suzuki, Naoyuki Taniguchi, Akemi Suzuki

    研究成果: ジャーナルへの寄稿学術論文査読

    25 被引用数 (Scopus)

    抄録

    High-sensitivity capillary electrophoresis-electrospray ionization quadrupole ion trap time-of-flight mass spectrometry (CE-ESI-QIT-TOF MS) was developed to structurally characterize four kinds of pyridylaminated (PA) oligosaccharides, i.e., lactose (Lac)-PA, globotriose (Gb3)-PA, globotetraose (Gb4)-PA, and IV3 αGalNAc-Gb 4 (Forssman antigen)-PA, derived from neutral glycosphingolipids. The CE-MS system included the head-column field-amplified sample stacking (HC-FASS) method for effective sample injection into a capillary column in CE, a sheathless interface between CE and a mass spectrometer, and MS and tandem MS (MS2) measurements with narrow mass range repeated high-speed switching. The total sensitivity of the developed CE-MS system was about 20 000 times higher than that of the conventional CE-MS system consisting of pressure injection, a sheath-flow interface, and a wide mass range measurement. The MS and MS2 spectra of the four PA-oligosaccharides at a concentration of 25 amol/μL in mixtures (each 250 amol/10 μL in a tube) clearly showed protonated molecular ions ([M + H]+) and the fragment ions responsible for the sequential elimination of saccharides. The developed CE-MS system is a powerful method for the structural characterization of glycosphingolipids extracted from very small amounts of biological materials and could be extended to the structural characterization of oligosaccharides derived from glycoproteins.

    本文言語英語
    ページ(範囲)7859-7865
    ページ数7
    ジャーナルAnalytical Chemistry
    85
    16
    DOI
    出版ステータス出版済み - 20-08-2013

    All Science Journal Classification (ASJC) codes

    • 分析化学

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