Analytical Chemistry
Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography
Wicht Kristina
1
,
Baert Mathijs
1
,
Schipperges Sonja
2
,
Von Doehren Norwin
3
,
Desmet G.
4
,
Van Geem K. M.
5
,
De Villiers André
6
,
Lynen Frédéric
1
2
Agilent Technologies, Hewlett Packard Street 8, D-76337 Waldbronn, Germany
|
3
Agilent Technologies, Netherlands BV, NL-4330 EA Middelburg, Netherlands
|
4
Department of Chemical Engineering, Vrije Universiteit Brussel, Pleinlaan 2, B-1050 Brussel, Belgium
|
Publication type: Journal Article
Publication date: 2022-11-28
Journal:
Analytical Chemistry
Quartile SCImago
Q1
Quartile WOS
Q1
Impact factor: 7.4
ISSN: 00032700, 15206882, 21542686
Abstract
In comprehensive two-dimensional liquid chromatography (LC × LC), solvents of high eluotropic strength are frequently used in the first dimension (1D), which lead to peak broadening in the second dimension (2D). In the majority of the current LC × LC column combinations, analytes are less than optimally refocused upon transfer to the second column, which negatively affects sensitivity. Furthermore, the typical combination of 1 or 2.1 mm columns in the 1D paired with a 3 mm (or broader) column in the 2D leads to at least a 9- or 4-fold dilution and a corresponding loss of sensitivity when using concentration-sensitive detectors. This occurs due to the enhanced radial dilution of the analytes in a broader column, while the sensitivity problem is further exacerbated in LC × LC due to the high flow operated 2D. In this paper, we introduce a solution to neutralize and inverse this dilution problem through a reconcentrating solution using temperature-responsive liquid chromatography (TRLC) in the 1D, which is a purely aqueous separation mode. Full solute refocusing at the 2D column head is thereby obtained when TRLC is combined with reversed-phase liquid chromatography (RPLC). This is shown for the combination of a 2.1 mm I.D. TRLC column with decreasing RPLC column diameters (3-2.1-1 mm) operated at the same linear velocities, hence a resulting decrease in dilution, respectively. Ultraviolet (UV) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) detection were used to determine the experimental detection limits. Sensitivity improvements with UV detection were somewhat lower than expected, but represent ∼1.5- and 3-fold sensitivity enhancement when using a 1 mm I.D. column compared to 2.1 or 3 mm I.D. columns in the 2D, respectively. This is attributed to extra-column dispersion and the poorer performance of 1 mm I.D. columns. A major benefit of the use of 1 mm I.D. columns in the 2D is that it allows split-free coupling of 2D effluent with ESI-MS (at 450 μL/min), making the coupling robust and simple. When using ESI-MS even better, albeit more variable, sensitivity enhancements were obtained on the narrower columns. The benefits of the methodology are demonstrated for paraben test solutes and for phenolic compounds in a blueberry extract by TRLC × RPLC-UV-ESI-TOF-MS.
Citations by journals
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1
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Chinese Herbal Medicines
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Chinese Herbal Medicines
1 publication, 50%
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Journal of Cleaner Production
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Journal of Cleaner Production
1 publication, 50%
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1
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Citations by publishers
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1
2
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Elsevier
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Elsevier
2 publications, 100%
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1
2
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- We do not take into account publications that without a DOI.
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- Statistics recalculated weekly.
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Wicht K. et al. Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography // Analytical Chemistry. 2022.
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Wicht K., Baert M., Schipperges S., Von Doehren N., Desmet G., Van Geem K. M., De Villiers A., Lynen F. Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography // Analytical Chemistry. 2022.
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TY - JOUR
DO - 10.1021/acs.analchem.2c03300
UR - https://doi.org/10.1021%2Facs.analchem.2c03300
TI - Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography
T2 - Analytical Chemistry
AU - Wicht, Kristina
AU - Baert, Mathijs
AU - Schipperges, Sonja
AU - Von Doehren, Norwin
AU - Desmet, G.
AU - Van Geem, K. M.
AU - De Villiers, André
AU - Lynen, Frédéric
PY - 2022
DA - 2022/11/28 00:00:00
PB - American Chemical Society (ACS)
SN - 0003-2700
SN - 1520-6882
SN - 2154-2686
ER -
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@article{2022_Wicht,
author = {Kristina Wicht and Mathijs Baert and Sonja Schipperges and Norwin Von Doehren and G. Desmet and K. M. Van Geem and André De Villiers and Frédéric Lynen},
title = {Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography},
journal = {Analytical Chemistry},
year = {2022},
publisher = {American Chemical Society (ACS)},
month = {nov},
url = {https://doi.org/10.1021%2Facs.analchem.2c03300},
doi = {10.1021/acs.analchem.2c03300}
}