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Efficient analysis of oligosaccharide‐malononitrile derivatives by on‐line capillary liquid chromatography/electrospray ionization mass spectrometry
Author(s) -
Ahn Yeong Hee,
Yoo Jong Shin
Publication year - 1999
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/(sici)1097-0231(19990530)13:10<855::aid-rcm558>3.0.co;2-g
Subject(s) - malononitrile , chemistry , derivatization , chromatography , oligosaccharide , mass spectrometry , electrospray ionization , organic chemistry , catalysis
Analyses of oligosaccharide‐malononitrile derivatives, which were obtained from the reactions of oligosaccharides with malononitrile under aqueous basic conditions, were conducted by on‐line capillary liquid chromatography/electrospray ionization mass spectrometry in negative‐ion mode. Among a variety of base catalysts for the derivatization of a oligosaccharide to its malononitrile derivative, sodium hydroxide gave the best result, rather than an amine base, with a rapid and clean conversion. The malononitrile derivative of maltoheptaose was detected with good peak shape at the 20 attomol level by selected ion monitoring. Especially in the analysis of multi‐component mixtures of oligosaccharide derivatives, addition of crotonaldehyde to the sample solution for the conversion of excess malononitrile to a non‐ionizable and more volatile compound, prior to the injection of sample onto the column, greatly improved the chromatographic resolution and peak symmetry of each oligosaccharide‐malononitrile derivative. The order of migration of oligosaccharide‐malononitrile derivatives on an aminopropylsilyl column followed the size of the carbohydrate moiety. Copyright © 1999 John Wiley & Sons, Ltd.