Fast CE for combinatorial catalysis

Michael C. Breadmore*, Richard Hodgson, Danielle F. Kennedy, Barbara A. Messerle

*Corresponding author for this work

Research output: Contribution to journalArticle

3 Citations (Scopus)

Abstract

Two solvent-modified MEKC methods were developed for the quantitative analysis of heterocyclic amines synthesised using intramolecular ring closure via catalysed hydroamination. The first method was capable of resolving six of the amines (precursors and products) with a sample-to-sample injection time of 2 min employing a 20 mM borate buffer, pH 9.2 with 20 mM SDS and 5% v/v n-butanol (n-BuOH). A second low-pH method using 20 mM phosphate buffer, 100 mm SDS, 5% v/v n-BuOH and 20% v/v iso-propanol (i-PrOH) was able to resolve an additional pair of compounds with a sample-to-sample time of 3.5 min. Application of the first method to the analysis of a sample containing catalyst as well as amines placed directly in a 96-well plate showed excellent performance, with migration time and peak height and area reproducibility being less than 0.9 and 9.6%, respectively. The quantity of conversion by catalyst was calculated to be 68 ± 7%, which was in excellent agreement with the 67 ± 5% obtained by more conventional 1H NMR experiments, with the added advantage that this method is also cheaper, quicker and more amendable to high-throughput screening of combinatorial libraries.

Original languageEnglish
Pages (from-to)491-498
Number of pages8
JournalElectrophoresis
Volume29
Issue number2
DOIs
Publication statusPublished - Jan 2008
Externally publishedYes

    Fingerprint

Cite this

Breadmore, M. C., Hodgson, R., Kennedy, D. F., & Messerle, B. A. (2008). Fast CE for combinatorial catalysis. Electrophoresis, 29(2), 491-498. https://doi.org/10.1002/elps.200700220