Analysis of organic reactions by thin layer chromatography combined with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

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 c...

Full description

Saved in:
Bibliographic Details
Published in:Rapid communications in mass spectrometry 1998-01, Vol.12 (20), p.1475-1484
Main Authors: Hilaire, Phaedria M. St, Cipolla, Laura, Tedebark, Ulf, Meldal, Morten
Format: Article
Language:English
Subjects:
Carbohydrates - chemistry
Chemistry, Organic - instrumentation
Chromatography, Thin Layer
Metals - chemistry
Molecular Conformation
Molecular Weight
Peptides - chemistry
Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary: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.
ISSN:0951-4198
1097-0231
DOI:10.1002/(SICI)1097-0231(19981030)12:20<1475::AID-RCM365>3.0.CO;2-F