Very high pressure liquid chromatography using fully porous particles: Quantitative analysis of fast gradient separations without post-run times

Stankovich, Joseph J., Gritti, Fabrice, Stevenson, Paul G., Beaver, Lois Ann and Guiochon, Georges 2014, Very high pressure liquid chromatography using fully porous particles: Quantitative analysis of fast gradient separations without post-run times, Journal of chromatography A, vol. 1324, pp. 155-163, doi: 10.1016/j.chroma.2013.11.036.

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Title Very high pressure liquid chromatography using fully porous particles: Quantitative analysis of fast gradient separations without post-run times
Author(s) Stankovich, Joseph J.
Gritti, Fabrice
Stevenson, Paul G.ORCID iD for Stevenson, Paul G. orcid.org/0000-0001-6780-6859
Beaver, Lois Ann
Guiochon, Georges
Journal name Journal of chromatography A
Volume number 1324
Start page 155
End page 163
Total pages 9
Publisher Elsevier
Place of publication Amsterdam, The Netherlands
Publication date 2014-01
ISSN 0021-9673
1873-3778
Keyword(s) very high pressure liquid chromatography (VHPLC)
constant pressure gradient elution
constant flow rate gradient elution
thermal equilibrium
Summary Using a column packed with fully porous particles, four methods for controlling the flow rates at which gradient elution runs are conducted in very high pressure liquid chromatography (VHPLC) were tested to determine whether reproducible thermal conditions could be achieved, such that subsequent analyses would proceed at nearly the same initial temperature. In VHPLC high flow rates are achieved, producing fast analyses but requiring high inlet pressures. The combination of high flow rates and high inlet pressures generates local heat, leading to temperature changes in the column. Usually in this case a post-run time is input into the analytical method to allow the return of the column temperature to its initial state. An alternative strategy involves operating the column without a post-run equilibration period and maintaining constant temperature variations for subsequent analysis after conducting one or a few separations to bring the column to a reproducible starting temperature. A liquid chromatography instrument equipped with a pressure controller was used to perform constant pressure and constant flow rate VHPLC separations. Six replicate gradient separations of a nine component mixture consisting of acetophenone, propiophenone, butyrophenone, valerophenone, hexanophenone, heptanophenone, octanophenone, benzophenone, and acetanilide dissolved in water/acetonitrile (65:35, v/v) were performed under various experimental conditions: constant flow rate, two sets of constant pressure, and constant pressure operation with a programmed flow rate. The relative standard deviations of the response factors for all the analytes are lower than 5% across the methods. Programming the flow rate to maintain a fairly constant pressure instead of using instrument controlled constant pressure improves the reproducibility of the retention times by a factor of 5, when plotting the chromatograms in time.
Language eng
DOI 10.1016/j.chroma.2013.11.036
Field of Research 030108 Separation Science
Socio Economic Objective 970103 Expanding Knowledge in the Chemical Sciences
HERDC Research category C1.1 Refereed article in a scholarly journal
Grant ID DE-FG05-88-ER-13869
Copyright notice ©2014, Elsevier
Persistent URL http://hdl.handle.net/10536/DRO/DU:30065443

Document type: Journal Article
Collection: School of Life and Environmental Sciences
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Created: Thu, 21 Aug 2014, 07:48:45 EST by Paul Stevenson

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