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Analysis of organic reactions by thin layer chromatography combined with matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry
Author(s) -
Hilaire Phaedria M. St.,
Cipolla Laura,
Tedebark Ulf,
Meldal Morten
Publication year - 1998
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(19981030)12:20<1475::aid-rcm365>3.0.co;2-f
Subject(s) - chemistry , mass spectrometry , analyte , chromatography , matrix assisted laser desorption/ionization , time of flight mass spectrometry , analytical chemistry (journal) , desorption , matrix (chemical analysis) , thin layer chromatography , ion suppression in liquid chromatography–mass spectrometry , ionization , ion , organic chemistry , liquid chromatography–mass spectrometry , adsorption
Abstract The products of a wide variety of organic reactions were rapidly identified by their masses through a combination of thin layer chromatography (TLC) and matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOFMS). Crude mixtures of peptides and glycopeptides, complex carbohydrate reactions, and a classical organic reaction were analysed using the following standard protocol. The components of the reaction mixtures were first separated on the TLC plate, scraped off, extracted and analysed by MALDI‐TOFMS. The technique used is easy and applicable to most organic reactions, becoming a very powerful technique in reaction optimization once composition and identity of TLC spots have been established by MS. Moreover, the TLC/MALDI‐TOFMS method was used to identify low molecular weight compounds with masses within the matrix region (100–500 u), a goal which is normally difficult to achieve. We successfully detected low molecular weight compounds by suppression of the matrix peaks using a relatively low matrix:analyte ratio (15:1 or lower). Doping both matrix and analyte solutions with [Cs] + ions resulted in suppression of both [Na] + and [K] + peaks, thus enhancing the spectral signals and making identification of low molecular weight compounds more facile. © 1998 John Wiley & Sons, Ltd.