Skip to main content

Lund University Publications

LUND UNIVERSITY LIBRARIES

On the fractionation of lignin oligomers by stepwise gradient reversed-phase liquid chromatography

Papp, Daniel LU and Sandahl, Margareta LU (2024) In Journal of chromatography. A 1737.
Abstract
With the increased interest in lignin valorization, the analytical
challenge to separate a complex mixture of a vast number of phenolics
has made chromatography an indispensable step in lignin analysis.
High-resolution separations, such as gas chromatography, reversed-phase
liquid chromatography and supercritical fluid chromatography have
typically been targeting low-molecular-weight compounds, while larger
lignin oligomers have received less attention. These compounds have
proven to be difficult to separate due to the inherent complexity of the
high-molecular-weight fraction of lignins, in fact, even high-resolving
linear reversed-phase gradients elute them as one wide zone. To tackle
... (More)
With the increased interest in lignin valorization, the analytical
challenge to separate a complex mixture of a vast number of phenolics
has made chromatography an indispensable step in lignin analysis.
High-resolution separations, such as gas chromatography, reversed-phase
liquid chromatography and supercritical fluid chromatography have
typically been targeting low-molecular-weight compounds, while larger
lignin oligomers have received less attention. These compounds have
proven to be difficult to separate due to the inherent complexity of the
high-molecular-weight fraction of lignins, in fact, even high-resolving
linear reversed-phase gradients elute them as one wide zone. To tackle
this, in this study we show that a crude fractionation of lignin
oligomers can be achieved by applying stepwise reversed-phase gradients.
A commonly employed reversed-phase system with water:acetonitrile
mobile phase is evaluated for this task. Special attention was devoted
to uncovering the molecular level explanation of the retention
phenomenon. Our results indicate that separation is mainly governed by
reversed-phase retention phenomena without any major exclusion or
viscosity-related effects, shown by great fits to linear retention
models (R2avg = 0.9599 for five different
oligomers) and apparent differences in retentivity between different
stationary phases. The influence of the gradient shape was demonstrated
by the comparison of stepwise gradients with different number and
frequency of steps, leading to the conclusion that gradients with a low
number of steps yield fewer, but better resolved fractions, while finer
multi-step gradients can be used to distinguish more fractions. (Less)
Please use this url to cite or link to this publication:
author
and
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Journal of chromatography. A
volume
1737
article number
465458
pages
6 pages
publisher
Elsevier
external identifiers
  • pmid:39490197
  • scopus:85207240870
ISSN
0021-9673
DOI
10.1016/j.chroma.2024.465458
project
Addressing the challenges of lignin oligomer analysis by liquid-based separation techniques
language
English
LU publication?
yes
id
9ed21c3a-e1d2-43c7-915f-7d27303fd7e7
date added to LUP
2024-11-17 20:09:30
date last changed
2025-04-04 14:06:21
@article{9ed21c3a-e1d2-43c7-915f-7d27303fd7e7,
  abstract     = {{With the increased interest in lignin valorization, the analytical <br>
challenge to separate a complex mixture of a vast number of phenolics <br>
has made chromatography an indispensable step in lignin analysis. <br>
High-resolution separations, such as gas chromatography, reversed-phase <br>
liquid chromatography and supercritical fluid chromatography have <br>
typically been targeting low-molecular-weight compounds, while larger <br>
lignin oligomers have received less attention. These compounds have <br>
proven to be difficult to separate due to the inherent complexity of the<br>
 high-molecular-weight fraction of lignins, in fact, even high-resolving<br>
 linear reversed-phase gradients elute them as one wide zone. To tackle <br>
this, in this study we show that a crude fractionation of lignin <br>
oligomers can be achieved by applying stepwise reversed-phase gradients.<br>
 A commonly employed reversed-phase system with water:acetonitrile <br>
mobile phase is evaluated for this task. Special attention was devoted <br>
to uncovering the molecular level explanation of the retention <br>
phenomenon. Our results indicate that separation is mainly governed by <br>
reversed-phase retention phenomena without any major exclusion or <br>
viscosity-related effects, shown by great fits to linear retention <br>
models (<em>R</em><sup>2</sup><sub>avg</sub> = 0.9599 for five different<br>
 oligomers) and apparent differences in retentivity between different <br>
stationary phases. The influence of the gradient shape was demonstrated <br>
by the comparison of stepwise gradients with different number and <br>
frequency of steps, leading to the conclusion that gradients with a low <br>
number of steps yield fewer, but better resolved fractions, while finer <br>
multi-step gradients can be used to distinguish more fractions.}},
  author       = {{Papp, Daniel and Sandahl, Margareta}},
  issn         = {{0021-9673}},
  language     = {{eng}},
  month        = {{11}},
  publisher    = {{Elsevier}},
  series       = {{Journal of chromatography. A}},
  title        = {{On the fractionation of lignin oligomers by stepwise gradient reversed-phase liquid chromatography}},
  url          = {{http://dx.doi.org/10.1016/j.chroma.2024.465458}},
  doi          = {{10.1016/j.chroma.2024.465458}},
  volume       = {{1737}},
  year         = {{2024}},
}