Improving peak shapes with counter gradients in two-dimensional high performance liquid chromatography

Stevenson, Paul G., Bassanese, Danielle N., Conlan, Xavier A. and Barnett, Neil W 2014, Improving peak shapes with counter gradients in two-dimensional high performance liquid chromatography, Journal of chromatography A, vol. 1337, pp. 147-154, doi: 10.1016/j.chroma.2014.02.051.

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Title Improving peak shapes with counter gradients in two-dimensional high performance liquid chromatography
Author(s) Stevenson, Paul G.ORCID iD for Stevenson, Paul G.
Bassanese, Danielle N.ORCID iD for Bassanese, Danielle N.
Conlan, Xavier A.ORCID iD for Conlan, Xavier A.
Barnett, Neil W
Journal name Journal of chromatography A
Volume number 1337
Start page 147
End page 154
Total pages 8
Publisher Elsevier
Place of publication Amsterdam, The Netherlands
Publication date 2014-04
ISSN 0021-9673
Keyword(s) two-dimensional high performance liquid chromatography
natural product separations
column efficiency
solvent strength
counter gradient
Summary To achieve the greatest peak capacity in two-dimensional high performance liquid chromatography (2D-HPLC) a gradient should be operated in both separation dimensions. However, it is known that when an injection solvent that is stronger than the initial mobile phase composition is deleterious to peak performance, thus causing problems when cutting a portion from one gradient into another. This was overcome when coupling hydrophilic interaction with reversed phase chromatography by introducing a counter gradient that changed the solvent strength of the second dimension injection. It was found that an injection solvent composition of 20% acetonitrile in water gave acceptable results in one-dimensional simulations with an initial composition of 5% acetonitrile. When this was transferred to a 2D-HPLC separation of standards it was found that a marked improvement in peak shape was gained for the moderately retained analytes (phenol and dimethyl phthalate), some improvement for the weakly retained caffeine and very little change for the strongly retained n-propylbenzene and anthracene which already displayed good chromatographic profiles. This effect was transferred when applied to a 2D-HPLC separation of a coffee extract where the indecipherable retention profile was transformed to a successful application multidimensional chromatography with peaks occupying 71% of the separation space according to the geometric approach to factor analysis.
Language eng
DOI 10.1016/j.chroma.2014.02.051
Field of Research 030108 Separation Science
Socio Economic Objective 970103 Expanding Knowledge in the Chemical Sciences
HERDC Research category C1 Refereed article in a scholarly journal
Copyright notice ©2014, Elsevier
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Created: Tue, 18 Feb 2014, 07:19:43 EST by Paul Stevenson

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