Abstract
The conversion of lignin to potentially high-value low molecular weight compounds often results in complex mixtures of monomeric and oligomeric compounds. In this study, a method for the quantitative and qualitative analysis of 40 lignin-derived compounds using ultra-high-performance supercritical fluid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPSFC/QTOF-MS) has been developed. Seven different columns were explored for maximum selectivity. Makeup solvent composition and ion source settings were optimised using a D-optimal design of experiment (DoE). Differently processed lignin samples were analysed and used for the method validation. The new UHPSFC/QTOF-MS method showed good separation of the 40 compounds within only 6-min retention time, and out of these, 36 showed high ionisation efficiency in negative electrospray ionisation mode.Graphical abstractA rapid and selective method for the quantitative and qualitative analysis of 40 lignin-derived compounds using ultra-high-performance supercritical fluid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPSFC/QTOF-MS)
Highlights
Lignin is a complex heterogeneous biopolymer containing differently substituted phenylpropanoid units, with the three basic building blocks being p-hydroxyphenyl (H), guaiacyl (G) and syringyl (S) [1]
We have previously shown that Supercritical fluid chromatography (SFC) is a promising technique for the analysis of lignin-derived compounds [18]
We are extending this approach to a broader range of phenolics by exploiting seven different SFC columns with modern stationary phase technology and high-resolution MS (HRMS) detection
Summary
Lignin is a complex heterogeneous biopolymer containing differently substituted phenylpropanoid units, with the three basic building blocks being p-hydroxyphenyl (H), guaiacyl (G) and syringyl (S) [1]. A necessary process in successful lignin valorisation is the depolymerisation of lignin into low molecular weight units, which can be further processed into several value-added compounds [2]. Gas chromatography (GC) with flame ionisation detection (FID) and mass spectrometry (MS) detection has, for long, been the dominating technique for monitoring of lignin depolymerisation [3, 4]. The reasons for this have mainly been the higher resolution, easier coupling with MS and lower costs, compared to LC-based techniques [5]. A disadvantage of GC over LC is the need for a derivatisation step prior to analysis, which will increase the analysis time and may result in insufficient and discriminative derivatisation that may compromise the quality of the results [6]
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