TY - JOUR
T1 - Structural characterization of pyridylaminated oligosaccharides derived from neutral glycosphingolipids by high-sensitivity capillary electrophoresis-mass spectrometry
AU - Ito, Emi
AU - Nakajima, Kazuki
AU - Waki, Hiroaki
AU - Miseki, Kozo
AU - Shimada, Takashi
AU - Sato, Taka Aki
AU - Kakehi, Kazuaki
AU - Suzuki, Minoru
AU - Taniguchi, Naoyuki
AU - Suzuki, Akemi
PY - 2013/8/20
Y1 - 2013/8/20
N2 - 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.
AB - 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.
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U2 - 10.1021/ac401460f
DO - 10.1021/ac401460f
M3 - Article
C2 - 23931631
AN - SCOPUS:84882686561
SN - 0003-2700
VL - 85
SP - 7859
EP - 7865
JO - Analytical Chemistry
JF - Analytical Chemistry
IS - 16
ER -