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Licensed Unlicensed Requires Authentication Published by De Gruyter April 27, 2022

A tailored fast thioacidolysis method incorporating multi-reaction monitoring mode of GC-MS for higher sensitivity on lignin monomer quantification

  • Linjie Yang , Jiangli Wang , Chen Wang , Fengxia Yue ORCID logo EMAIL logo and Fachuang Lu EMAIL logo
From the journal Holzforschung


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.

Corresponding authors: Fengxia Yue, State Key Laboratory of Pulp and Paper Engineering, School of Light Industry and Engineering, South China University of Technology, Guangzhou 510640, China, E-mail: ; and Fachuang Lu, State Key Laboratory of Pulp and Paper Engineering, School of Light Industry and Engineering, South China University of Technology, Guangzhou 510640, China; and Department of Biochemistry and Great Lakes Bioenergy Research Center, The Wisconsin Energy Institute, University of Wisconsin, Madison, WI 53726, USA, E-mail:

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


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.

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. 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).

  3. Conflict of interest statement: The authors declare that they have no conflicts of interest regarding this article.


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Supplementary Material

The online version of this article offers supplementary material (

Received: 2021-11-10
Accepted: 2022-03-18
Published Online: 2022-04-27
Published in Print: 2022-07-26

© 2022 Walter de Gruyter GmbH, Berlin/Boston

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