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Increasing Flexibility in Two-Dimensional Liquid Chromatography by Pulsed Elution of the First Dimension: A Proof of Concept

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    Increasing Flexibility in Two-Dimensional Liquid Chromatography by Pulsed Elution of the First Dimension: A Proof of Concept
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    † Department of Plant and Environmental Sciences, Faculty of Science, University of Copenhagen, Thorvaldsensvej 40, DK-1871 Frederiksberg C, Denmark
    ‡ Haldor Topsoe A/S, Haldor Topsøes Allé 1, DK-2800 Kongens Lyngby, Denmark
    § Waters Corporation, 34 Maple Street, Milford, Massachusetts 01757, United States
    *E-mail: [email protected]
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    Analytical Chemistry

    Cite this: Anal. Chem. 2017, 89, 17, 8723–8730
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    https://doi.org/10.1021/acs.analchem.7b00758
    Published July 31, 2017
    Copyright © 2017 American Chemical Society
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    Abstract

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    This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension is kept in a no-elution state using low eluent strength. The eluate from the first dimension is actively modulated using trap columns and subsequently analyzed in the second dimension. We demonstrate that by tuning the length and eluotropic strength of the pulses, peaks with retention factors in water, kw, above 150 can be manipulated to elute in 3–4 pulses. The no-elution state can be kept for 1–10 min with only minor changes as to which and how many pulses the peaks elute in. Pulsed-elution 2D-LC combined with active modulation tackles three of the main challenges encountered in 2D-LC and specifically online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity was 4018 for a 540 min analysis and 4610 for a 1040 min analysis.

    Copyright © 2017 American Chemical Society

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    Supporting Information

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.analchem.7b00758.

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    Cited By

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    This article is cited by 21 publications.

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    Analytical Chemistry

    Cite this: Anal. Chem. 2017, 89, 17, 8723–8730
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.analchem.7b00758
    Published July 31, 2017
    Copyright © 2017 American Chemical Society
    Request reuse permissions

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