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A simple protocol to determine lignin S/G ratio in plants by UHPLC-MS

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Abstract

A simple extraction protocol and an ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS) method for the determination of the syringyl/guaiacyl (S/G) ratio in lignin is reported herein. The method was entirely developed using stems of three Eucalyptus species, which were hydrolyzed with NaOH and partitioned with ethyl ether; vanillin (from the G monomer) and syringaldehyde (from S monomer) were quantified. The S/G ratios obtained were comparable to those usually reported for eucalyptus. The data for one of the eucalyptus species were compared with those obtained with a widely accepted method using thioacidolysis and gas chromatography-mass spectrometry (GC-MS). The method was also applied to sugarcane and showed to be reliable. The yield of the NaOH hydrolysis of the monolignols ranged from 89.94 to 95.69 %, with more than 77.12 % of recuperation in the liquid-liquid extraction. The whole analytical procedure was validated, achieving results with less than 4.38 % of variation. The lowest LOD and LOQ were 0.01 and 0.05 μg/mL, respectively. In addition, the method combines reliability and a fast and direct quantification.

A simple extraction protocol and UHPLC-MS method for the determination of the syringyl/guaiacyl (S/G) ratio in lignin

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Acknowledgments

We thank Marcos N. Eberlin for the FT-ICR-MS analysis of the hydrolysis products. This work was supported by the Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) grants no. 2008/58035-6 and 2011/51949-5. PM thanks Conselho Nacional de Pesquisa—Brazil (CNPq) for a research fellowship; JBM and GAB thank FAPESP grants no. 2013/21306-0 and 2012/21395-0, respectively, for a doctoral fellowship.

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Authors and Affiliations

  1. Department of Plant Biology, Institute of Biology, State University of Campinas, UNICAMP, 13083-970, Campinas, São Paulo, Brazil

    Joao Benhur Mokochinski, Eduardo Kiyota, Letícia Marrone de Souza, Paulo Mazzafera & Alexandra Christine Helena Frankland Sawaya

  2. ThoMSon Mass Spectrometry Laboratory, Institute of Chemistry, State University of Campinas, UNICAMP, 13083-970, Campinas, São Paulo, Brazil

    Giovana Anceski Bataglion

Authors
  1. Joao Benhur Mokochinski
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  2. Giovana Anceski Bataglion
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  3. Eduardo Kiyota
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  4. Letícia Marrone de Souza
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  5. Paulo Mazzafera
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  6. Alexandra Christine Helena Frankland Sawaya
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Correspondence to Alexandra Christine Helena Frankland Sawaya.

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Mokochinski, J.B., Bataglion, G.A., Kiyota, E. et al. A simple protocol to determine lignin S/G ratio in plants by UHPLC-MS. Anal Bioanal Chem 407, 7221–7227 (2015). https://doi.org/10.1007/s00216-015-8886-9

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  • DOI: https://doi.org/10.1007/s00216-015-8886-9

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