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Enhancing the Possibilities of Comprehensive Two-Dimensional Liquid Chromatography through Hyphenation of Purely Aqueous Temperature-Responsive and Reversed-Phase Liquid Chromatography

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    Enhancing the Possibilities of Comprehensive Two-Dimensional Liquid Chromatography through Hyphenation of Purely Aqueous Temperature-Responsive and Reversed-Phase Liquid Chromatography
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    • Mathijs Baert
      Mathijs Baert
      Separation Science Group, Department of Organic and Macromolecular Chemistry, Ghent University, Krijgslaan 281 S4bis, B-9000 Ghent, Belgium
      More by Mathijs Baert
    • Steven Martens
      Steven Martens
      Polymer Chemistry Research Group, Centre of Macromolecular Chemistry (CMaC), Department of Organic and Macromolecular Chemistry, Ghent University, Krijgslaan 281 S4bis, B-9000 Ghent, Belgium
      More by Steven Martens
    • Gert Desmet
      Gert Desmet
      Department of Chemical Engineering, Vrije Universiteit Brussel, Pleinlaan 2, 1050 Brussel, Belgium
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      Orcidhttp://orcid.org/0000-0002-6430-3962
    • André de Villiers
      André de Villiers
      Department of Chemistry and Polymer Science, Stellenbosch University, Private Bag X1, Matieland, Stellenbosch 7602, South Africa
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    • Filip Du Prez
      Filip Du Prez
      Polymer Chemistry Research Group, Centre of Macromolecular Chemistry (CMaC), Department of Organic and Macromolecular Chemistry, Ghent University, Krijgslaan 281 S4bis, B-9000 Ghent, Belgium
      More by Filip Du Prez
      Orcidhttp://orcid.org/0000-0001-7727-4155
    • Frederic Lynen*
      Frederic Lynen
      Separation Science Group, Department of Organic and Macromolecular Chemistry, Ghent University, Krijgslaan 281 S4bis, B-9000 Ghent, Belgium
      *Tel: +32 (0) 9 264 9606; Fax: +32 (0) 9 264 4998; E-mail: [email protected]
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      Orcidhttp://orcid.org/0000-0002-4690-7690
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    Analytical Chemistry

    Cite this: Anal. Chem. 2018, 90, 8, 4961–4967
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    https://doi.org/10.1021/acs.analchem.7b04914
    Published March 18, 2018
    Copyright © 2018 American Chemical Society
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    Abstract

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    Comprehensive two-dimensional liquid chromatography (LC × LC) allows for substantial gains in theoretical peak capacity in the field of liquid chromatography. However, in practice, theoretical performance is rarely achieved due to a combination of undersampling, orthogonality, and refocusing issues prevalent in many LC × LC applications. This is intricately linked to the column dimensions, flow rates, and mobile-phase compositions used, where, in many cases, incompatible or strong solvents are introduced in the second-dimension (2D) column, leading to peak broadening and the need for more complex interfacing approaches. In this contribution, the combination of temperature-responsive (TR) and reversed-phase (RP) LC is demonstrated, which, due to the purely aqueous mobile phase used in TRLC, allows for complete and more generic refocusing of organic solutes prior to the second-dimension RP separation using a conventional 10-port valve interface. Thus far, this was only possible when combining other purely aqueous modes such as ion exchange or gel filtration chromatography with RPLC, techniques which are limited to the analysis of charged or high MW solutes, respectively. This novel TRLC × RPLC combination relaxes undersampling constraints and complete refocusing and therefore offers novel possibilities in the field of LC × LC including temperature modulation. The concept is illustrated through the TRLC × RPLC analysis of mixtures of neutral organic solutes.

    Copyright © 2018 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.7b04914.

    • Synthesis of temperature-responsive column; calculation of TRLC × RPLC peak capacity; supplementary information on the test mixture and steroid mixture (PDF)

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    Analytical Chemistry

    Cite this: Anal. Chem. 2018, 90, 8, 4961–4967
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.analchem.7b04914
    Published March 18, 2018
    Copyright © 2018 American Chemical Society
    Request reuse permissions

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