Isolation of κ-carrageenan oligosaccharides using ion-pair liquid chromatography -: characterisation by electrospray ionisation mass spectrometry in positive-ion mode

被引:26
作者
Antonopoulos, A
Favetta, P
Helbert, W
Lafosse, M
机构
[1] Univ Orleans, CNRS, UMR 6005, Inst Chim Organ & Analyt, F-45067 Orleans, France
[2] CNRS, Biol Stn, Lab Goemar, UMR 1931, F-29682 Roscoff, France
关键词
kappa-carrageenan; ion-pair liquid chromatography; electrospray ionisation mass spectrometry; evaporative light scattering detector; sulfated oligosaccharides;
D O I
10.1016/j.carres.2004.03.002
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
Oligo-kappa-carrageenans participate as elicitors in the cell-cell recognition process in marine plants. Analytical methods can be usefully applied to gain insight into the biochemistry of these biological processes. Therefore, enzymatically digested oligomers of kappa-carrageenans have been separated and isolated on a Spherisorb ODSI (250x4 mm i.d., particle size 5 mum) column using ion-pair liquid chromatography coupled with an evaporative light scattering detector. Heptylamine (5 mM, pH 4) has been selected as the ion-pairing agent and MeOH as the organic modifier in a gradient mode. Overloading the column with 1 mg of the mixture, the chromatographic mechanism presented adequate stability. The mobile phase of each isolated oligomer was evaporated and the residue was infused into an electrospray ionisation mass spectrometry (ESIMS) in positive-ion mode with 4:1 MeCN-water as mobile phase. Each ESIMS spectrum presented ions consisting of the oligomer attached with a number of heptylammonium ions depending on the molecule size. In addition, the different m/z values permitted direct detection of the oligomers in ESIMS positive-ion mode. The analytical method developed separated the oligomers up to dotriacontasaccharide. (C) 2004 Elsevier Ltd. All rights reserved.
引用
收藏
页码:1301 / 1309
页数:9
相关论文
共 44 条
[1]   Analysis of carrageenans by matrix-assisted laser desorption/ionization and electrospray ionization mass spectrometry.: I.: kappa-carrageenans [J].
Ackloo, S ;
Terlouw, JK ;
Ruttink, PJA ;
Burgers, PC .
RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 2001, 15 (14) :1152-1159
[2]   Comparative analysis of enzymatically digested κ-carrageenans, using liquid chromatography on ion-exchange and porous graphitic carbon columns coupled to an evaporative light scattering detector [J].
Antonopoulos, A ;
Herbreteau, B ;
Lafosse, M ;
Helbert, W .
JOURNAL OF CHROMATOGRAPHY A, 2004, 1023 (02) :231-238
[3]   IDENTIFICATION AND CHARACTERIZATION OF BIOLOGICAL PRECURSORS OF CARRAGEENANS BY C-13 NMR-SPECTROSCOPY [J].
BELLION, C ;
BRIGAND, G ;
PROME, JC ;
WELTI, D ;
BOCIEK, S .
CARBOHYDRATE RESEARCH, 1983, 119 (AUG) :31-48
[4]  
Bixler HJ, 1996, HYDROBIOLOGIA, V327, P35
[5]   The Chondrus crispus Acrochaete operculata host-pathogen association, a novel model in glycobiology and applied phycopathology [J].
Bouarab, K ;
Potin, P ;
Weinberger, F ;
Correa, J ;
Kloareg, B .
JOURNAL OF APPLIED PHYCOLOGY, 2001, 13 (02) :185-193
[6]   Sulfated oligosaccharides mediate the interaction between a marine red alga and its green algal pathogenic endophyte [J].
Bouarab, K ;
Potin, P ;
Correa, J ;
Kloareg, B .
PLANT CELL, 1999, 11 (09) :1635-1650
[7]  
Craigie J. S., 1990, BIOL RED ALGAE, P221
[8]   Carrageenan biotechnology [J].
De Ruiter, GA ;
Rudolph, B .
TRENDS IN FOOD SCIENCE & TECHNOLOGY, 1997, 8 (12) :389-395
[9]   Size exclusion chromatography/mass spectrometry applied to the analysis of polysaccharides [J].
Deery, MJ ;
Stimson, E ;
Chappell, CG .
RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 2001, 15 (23) :2273-2283
[10]   Negative-ion electrospray ionisation-mass spectrometry (ESI-MS) as a tool for analysing structural heterogeneity in kappa-carrageenan oligosaccharides [J].
Ekeberg, D ;
Knutsen, SH ;
Sletmoen, M .
CARBOHYDRATE RESEARCH, 2001, 334 (01) :49-59