Premium
Fast CE for combinatorial catalysis
Author(s) -
Breadmore Michael C.,
Hodgson Richard,
Kennedy Danielle F.,
Messerle Barbara A.
Publication year - 2008
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.200700220
Subject(s) - hydroamination , catalysis , chemistry , phosphate buffered saline , intramolecular force , solvent , boron , chromatography , reproducibility , combinatorial chemistry , analytical chemistry (journal) , organic chemistry
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 1 H NMR experiments, with the added advantage that this method is also cheaper, quicker and more amendable to high‐throughput screening of combinatorial libraries.