MALDI-TOF MS Analysis of Soluble PEG based Multi-step Synthetic Reaction Mixtures with Automated Detection of Reaction Failure

Macromolecules of tunable solubility, used to mimic inert insoluble materials while maintaining solution conditions, allowed the performance of efficient supported organic chemistry and facilitate in situ reaction monitoring. To satisfy the high throughput requirements of automated synthetic process...

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Bibliographic Details
Published inJournal of the American Society for Mass Spectrometry Vol. 16; pp. 670 - 678
Main Authors Enjalbal, Christine, Ribière, Patrice, Lamaty, Frédéric, Yadav-Bhatnagar, Neerja, Martinez, Jean, Aubagnac, Jean-Louis
Format Journal Article
LanguageEnglish
Published American Chemical Society 2005
Subjects
Chemical Sciences
Life Sciences
Material chemistry
Other
MALDI mass spectrometry
Automation
PEG
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Summary:Macromolecules of tunable solubility, used to mimic inert insoluble materials while maintaining solution conditions, allowed the performance of efficient supported organic chemistry and facilitate in situ reaction monitoring. To satisfy the high throughput requirements of automated synthetic processes, organic syntheses carried out on bifunctional polyethylene glycol polymers (PEG3400-OH) were monitored step-by-step by Matrix Assisted Laser Desorption Ionization - Time of flight Mass Spectrometry. A protocol was designed to control the ionization mechanism of such polymers exhibiting high affinity for alkali metal cations. Automated, rapid and reliable data interpretation was performed by an in-house developed visual basic application relying on the sodiated ion accurate monoisotopic mass measurement. The methodology was illustrated through the monitoring of a six-step synthetic scheme.
ISSN:1044-0305
1879-1123
DOI:10.1016/j.jasmas.2005.01.020