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Fast CE for combinatorial catalysis


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Breadmore, MC, Hodgson, R, Kennedy, DF and Messerle, BA 2008 , 'Fast CE for combinatorial catalysis' , Electrophoresis, vol. 29, no. 2 , pp. 491-498 , doi: 10.1002/elps.200700220.

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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.

Item Type: Article
Authors/Creators:Breadmore, MC and Hodgson, R and Kennedy, DF and Messerle, BA
Keywords: Catalysis • Combinatorial screening • Fast CE • High-throughput screening • Solvent modified MEKC
Journal or Publication Title: Electrophoresis
ISSN: 0173-0835
DOI / ID Number: 10.1002/elps.200700220
Additional Information:

Funded by:
Australian Research Council; Grant Number: DP0453223, DP0556759
University of New South Wales

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