Ultra-high-performance supercritical fluid chromatography with quadrupole-time-of-flight mass spectrometry (UHPSFC/QTOF-MS) for analysis of lignin-derived monomeric compounds in processed lignin samples.

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 abstract A 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).