Optimization of sample preparation conditions in the study of lignin by MALDI mass spectrometry method

T11N2

D.S. Kosyakov, N.V. Ul’yanovskii, E.A. Sorokina, N.S. Gorbova

In the present study the comparison of efficacy of six crystalline matrices, as well as their mixtures for MALDI of lignin is done, the effect of sample application technique and matrix/analyte ratio on the quality of the mass spectra is studied. It is established that the best results can be obtained when α-cyano-4-hydroxycinnamic and 2,5-dihydroxybenzoic acids, a well as 2,4,6-trihydroxyacetophenone are used as matrices, taken in 10–100-fold excess with respect to lignin and sequentially applied to the target in order «analyte–matrix– analyte». It is proposed for the first time to use ionic liquids as martices for obtaining of lignin MALDI mass spectra. It is shown that the ionic liquid N-tert-butyl-N-isopropyl-N-methylammonium α-cyano-4-hydroxycinnamate, forming a homogeneous solution with lignin gives substantially better results when compared with crystalline matrices in terms of intensity of the obtained mass spectra, and reproducibility. The structure of the MALDI mass spectra of dioxane lignin of fir caused by the predominance in the macromolecule units derived from α-guaiacylpropanone is analyzed.

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