Abstract
Thioacidolysis is widely used for lignin structural characterization by cleaving β-aryl ethers to release syringyl (S), guaiacyl (G), and p-hydroxyphenyl (H) monomers followed by GC analysis. However, the traditional thioacidolysis method requires tedious extraction steps with chlorinated solvent underlying harmful to health, limiting its efficiency and application. Herein, an improved thioacidolysis method with high sensitivity for the quantitation of lignin-derived monomers was developed. The improved protocol used a quick, streamlined procedure to recover the monomeric products using ethyl acetate as extracting solvent and MS detector in multi-reaction monitoring mode to enhance its ability to detect extremely low concentration (0.1 ppb with signal-to-noise higher than 2) of monomeric products. Additionally, a fast GC program was established to speed up the GC quantitation. Several representative lignocellulose samples, including gymnosperm, angiosperm, and poaceae, were used to test this tailored method. The results demonstrated that the ratios of lignin monomer compositions determined by this method were consistent with that of traditional procedure despite the slightly higher monomer yields measured. More importantly, this method uses non-chlorinated solvent for microscale extraction and requires no evaporation step for workup, which is a green and efficient way for the quantification of lignin monomer compositions.
Funding source: National Natural Science Foundation of China
Award Identifier / Grant number: 31770621
Award Identifier / Grant number: 31870560
Funding source: The DOE Great Lakes Bioenergy Research Center
Award Identifier / Grant number: DOE BER Office of Science DE-SC0018409
Acknowledgments
The authors are very grateful to Dr. Wenzhang Ma of Herbarium (KUN), Kunming Institute of Botany, Chinese Academy of Sciences for kindly providing the Polytrichum and Pogonatum proliferum samples.
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Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
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Research funding: The work was supported by the National Natural Science Foundation of China (31870560 and 31770621) and the DOE Great Lakes Bioenergy Research Center (DOE BER Office of Science, DE-SC0018409).
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Conflict of interest statement: The authors declare that they have no conflicts of interest regarding this article.
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