Rationale: Effective analytical techniques are needed to characterize lignin products for the generation of renewable carbon sources. Application of matrix-assisted laser desorption/ionization (MALDI) in lignin analysis is limited because of poor ionization efficiency. In this study, we explored the potential of cationization along with a 2,5-dihydroxyacetophenone (DHAP) matrix to characterize model lignin oligomers.
Methods: Synthesized lignin oligomers were analyzed using the developed MALDI method. Two matrix systems, DHAP and α-cyano-4-hydroxycinnamic acid (CHCA), and three cations (lithium, sodium, silver) were evaluated using a Bruker UltraFlextreme time-of-flight mass spectrometer. Instrumental parameters, cation concentration, matrix, sample concentrations, and sample spotting protocols were optimized for improved results.
Results: The DHAP/Li combination was effective for dimer analysis as lithium adducts. Spectra from DHP and ferric chloride oligomers showed improved signal intensities up to decamers (m/z 1823 for the FeCl system) and provided insights into differences in the oligomerization mechanism. Spectra from a mixed DHP oligomer system containing H, G, and S units showed contributions from all monolignols within an oligomer level (e.g. tetramer level).
Conclusions: The DHAP/Li method presented in this work shows promise to be an effective analytical tool for lignin analysis by MALDI and may provide a tool to assess lignin break-down efforts facilitating renewable products from lignin.
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