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Title: High-throughput prediction of eucalypt lignin syringyl/guaiacyl content using multivariate analysis: A comparison between mid-infrared, near-infrared, and Raman spectroscopies for model development

Abstract

Background: In order to rapidly and efficiently screen potential biofuel feedstock candidates for quintessential traits, robust high-throughput analytical techniques must be developed and honed. The traditional methods of measuring lignin syringyl/guaiacyl (S/G) ratio can be laborious, involve hazardous reagents, and/or be destructive. Vibrational spectroscopy can furnish high-throughput instrumentation without the limitations of the traditional techniques. Spectral data from mid-infrared, near-infrared, and Raman spectroscopies was combined with S/G ratios, obtained using pyrolysis molecular beam mass spectrometry, from 245 different eucalypt and Acacia trees across 17 species. Iterations of spectral processing allowed the assembly of robust predictive models using partial least squares (PLS). Results: The PLS models were rigorously evaluated using three different randomly generated calibration and validation sets for each spectral processing approach. Root mean standard errors of prediction for validation sets were lowest for models comprised of Raman (0.13 to 0.16) and mid-infrared (0.13 to 0.15) spectral data, while near-infrared spectroscopy led to more erroneous predictions (0.18 to 0.21). Correlation coefficients (r) for the validation sets followed a similar pattern: Raman (0.89 to 0.91), mid-infrared (0.87 to 0.91), and near-infrared (0.79 to 0.82). These statistics signify that Raman and mid-infrared spectroscopy led to the most accurate predictions of S/G ratiomore » in a diverse consortium of feedstocks. Conclusion: Eucalypts present an attractive option for biofuel and biochemical production. Given the assortment of over 900 different species of Eucalyptus and Corymbia, in addition to various species of Acacia, it is necessary to isolate those possessing ideal biofuel traits. This research has demonstrated the validity of vibrational spectroscopy to efficiently partition different potential biofuel feedstocks according to lignin S/G ratio, significantly reducing experiment and analysis time and expense while providing non-destructive, accurate, global, predictive models encompassing a diverse array of feedstocks.« less

Authors:
 [1];  [2];  [3];  [4];  [5];  [6];  [7]
+ Show Author Affiliations
  1. Univ. of Queensland, Lucias (Australia); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Sandia National Lab. (SNL-CA), Livermore, CA (United States)
  3. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); National Renewable Energy Lab. (NREL), Golden, CO (United States)
  4. Univ. of the Sunshine Coast and Queensland Dept. of Agriculture, Maroochydore, QLD (Australia)
  5. Southern Cross Univ., East Lismore, NSW (Australia)
  6. Univ. of Queensland, Lucias, QLD (Australia); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Sandia National Lab. (SNL-CA), Livermore, CA (United States)
  7. Univ. of Queensland, Lucias, QLD (Australia)
Publication Date:
Research Org.:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Biological and Environmental Research (BER). Biological Systems Science Division
OSTI Identifier:
1511400
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Accepted Manuscript
Journal Name:
Biotechnology for Biofuels
Additional Journal Information:
Journal Volume: 7; Journal Issue: 1; Journal ID: ISSN 1754-6834
Publisher:
BioMed Central
Country of Publication:
United States
Language:
English
Subject:
09 BIOMASS FUELS; 59 BASIC BIOLOGICAL SCIENCES; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Biomass; Raman spectroscopy; Near-infrared spectroscopy; Fourier-transform infrared spectroscopy; High-throughput; Multivariate analysis; Lignin S/G

Citation Formats

Lupoi, Jason S., Singh, Seema, Davis, Mark, Lee, David J., Shepherd, Merv, Simmons, Blake A., and Henry, Robert J. High-throughput prediction of eucalypt lignin syringyl/guaiacyl content using multivariate analysis: A comparison between mid-infrared, near-infrared, and Raman spectroscopies for model development. United States: N. p., 2014. Web. doi:10.1186/1754-6834-7-93.
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Lupoi, Jason S., Singh, Seema, Davis, Mark, Lee, David J., Shepherd, Merv, Simmons, Blake A., & Henry, Robert J. High-throughput prediction of eucalypt lignin syringyl/guaiacyl content using multivariate analysis: A comparison between mid-infrared, near-infrared, and Raman spectroscopies for model development. United States. https://doi.org/10.1186/1754-6834-7-93
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Lupoi, Jason S., Singh, Seema, Davis, Mark, Lee, David J., Shepherd, Merv, Simmons, Blake A., and Henry, Robert J. Tue . "High-throughput prediction of eucalypt lignin syringyl/guaiacyl content using multivariate analysis: A comparison between mid-infrared, near-infrared, and Raman spectroscopies for model development". United States. https://doi.org/10.1186/1754-6834-7-93. https://www.osti.gov/servlets/purl/1511400.
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@article{osti_1511400,
title = {High-throughput prediction of eucalypt lignin syringyl/guaiacyl content using multivariate analysis: A comparison between mid-infrared, near-infrared, and Raman spectroscopies for model development},
author = {Lupoi, Jason S. and Singh, Seema and Davis, Mark and Lee, David J. and Shepherd, Merv and Simmons, Blake A. and Henry, Robert J.},
abstractNote = {Background: In order to rapidly and efficiently screen potential biofuel feedstock candidates for quintessential traits, robust high-throughput analytical techniques must be developed and honed. The traditional methods of measuring lignin syringyl/guaiacyl (S/G) ratio can be laborious, involve hazardous reagents, and/or be destructive. Vibrational spectroscopy can furnish high-throughput instrumentation without the limitations of the traditional techniques. Spectral data from mid-infrared, near-infrared, and Raman spectroscopies was combined with S/G ratios, obtained using pyrolysis molecular beam mass spectrometry, from 245 different eucalypt and Acacia trees across 17 species. Iterations of spectral processing allowed the assembly of robust predictive models using partial least squares (PLS). Results: The PLS models were rigorously evaluated using three different randomly generated calibration and validation sets for each spectral processing approach. Root mean standard errors of prediction for validation sets were lowest for models comprised of Raman (0.13 to 0.16) and mid-infrared (0.13 to 0.15) spectral data, while near-infrared spectroscopy led to more erroneous predictions (0.18 to 0.21). Correlation coefficients (r) for the validation sets followed a similar pattern: Raman (0.89 to 0.91), mid-infrared (0.87 to 0.91), and near-infrared (0.79 to 0.82). These statistics signify that Raman and mid-infrared spectroscopy led to the most accurate predictions of S/G ratio in a diverse consortium of feedstocks. Conclusion: Eucalypts present an attractive option for biofuel and biochemical production. Given the assortment of over 900 different species of Eucalyptus and Corymbia, in addition to various species of Acacia, it is necessary to isolate those possessing ideal biofuel traits. This research has demonstrated the validity of vibrational spectroscopy to efficiently partition different potential biofuel feedstocks according to lignin S/G ratio, significantly reducing experiment and analysis time and expense while providing non-destructive, accurate, global, predictive models encompassing a diverse array of feedstocks.},
doi = {10.1186/1754-6834-7-93},
journal = {Biotechnology for Biofuels},
number = 1,
volume = 7,
place = {United States},
year = {Tue Jun 17 00:00:00 EDT 2014},
month = {Tue Jun 17 00:00:00 EDT 2014}
}
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Journal Article:
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Publisher's Version of Record
https://doi.org/10.1186/1754-6834-7-93
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Cited by: 30 works
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Figures / Tables:

Table 1 Table 1: Evaluation of literature multivariate models for lignin S/G prediction
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Works referenced in this record:

Bioenergy from plants and the sustainable yield challenge
journal, July 2008

Ultra Violet Resonance Raman Spectroscopy in Lignin Analysis: Determination of Characteristic Vibrations of p -Hydroxyphenyl, Guaiacyl, and Syringyl Lignin Structures
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Lignin monomer composition affects Arabidopsis cell-wall degradability after liquid hot water pretreatment
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  • DOI: 10.1186/1754-6834-3-27

Lignin content in natural Populus variants affects sugar release
journal, March 2011

  • Studer, M. H.; DeMartini, J. D.; Davis, M. F.
  • Proceedings of the National Academy of Sciences, Vol. 108, Issue 15, p. 6300-6305
  • DOI: 10.1073/pnas.1009252108

An overview of second generation biofuel technologies
journal, March 2010

Characterization of Woody and Herbaceous Biomasses Lignin Composition with 1064 nm Dispersive Multichannel Raman Spectroscopy
journal, August 2012

  • Lupoi, Jason S.; Smith, Emily A.
  • Applied Spectroscopy, Vol. 66, Issue 8
  • DOI: 10.1366/12-06621

Rapid determination of syringyl: Guaiacyl ratios using FT-Raman spectroscopy
journal, November 2011

  • Sun, Lan; Varanasi, Patanjali; Yang, Fan
  • Biotechnology and Bioengineering, Vol. 109, Issue 3
  • DOI: 10.1002/bit.24348

Genetic Variation in the Chemical Components of Eucalyptus globulus Wood
journal, July 2011

  • Stackpole, Desmond J.; Vaillancourt, René E.; Alves, Ana
  • G3: Genes|Genomes|Genetics, Vol. 1, Issue 2
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1064nm dispersive multichannel Raman spectroscopy for the analysis of plant lignin
journal, November 2011

  • Meyer, Matthew W.; Lupoi, Jason S.; Smith, Emily A.
  • Analytica Chimica Acta, Vol. 706, Issue 1
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Cellulosic Biofuels
journal, June 2009

Hydrogen Bonding in Lignin:  A Fourier Transform Infrared Model Compound Study
journal, September 2005

  • Kubo, Satoshi; Kadla, John F.
  • Biomacromolecules, Vol. 6, Issue 5
  • DOI: 10.1021/bm050288q

Evaluation of plant biomass resources available for replacement of fossil oil
journal, April 2010

Estimation of Aromatic Structure Contents in Hardwood Lignins from IR Absorption Spectra
journal, November 2013

Assessment of Lignocellulosic Biomass Using Analytical Spectroscopy: an Evolution to High-Throughput Techniques
journal, July 2013

Determining the influence of eucalypt lignin composition in paper pulp yield using Py-GC/MS
journal, August 2005

  • del Río, José C.; Gutiérrez, Ana; Hernando, Marina
  • Journal of Analytical and Applied Pyrolysis, Vol. 74, Issue 1-2
  • DOI: 10.1016/j.jaap.2004.10.010

Composition of non-woody plant lignins and cinnamic acids by Py-GC/MS, Py/TMAH and FT-IR
journal, May 2007

  • del Río, José C.; Gutiérrez, Ana; Rodríguez, Isabel M.
  • Journal of Analytical and Applied Pyrolysis, Vol. 79, Issue 1-2
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Development of the partial least squares models for the interpretation of the UV resonance Raman spectra of lignin model compounds
journal, January 2005

  • Saariaho, Anna-Maija; Argyropoulos, Dimitris S.; Jääskeläinen, Anna-Stiina
  • Vibrational Spectroscopy, Vol. 37, Issue 1
  • DOI: 10.1016/j.vibspec.2004.08.001

Identifying Softwoods and Hardwoods by Infrared Spectroscopy
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Characterization by Infrared Spectrometry of Lignins of Three Eucalyptus Species
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FT–Raman Investigation of Milled-Wood Lignins: Softwood, Hardwood, and Chemically Modified Black Spruce Lignins
journal, October 2011

  • Agarwal, Umesh P.; McSweeny, James D.; Ralph, Sally A.
  • Journal of Wood Chemistry and Technology, Vol. 31, Issue 4
  • DOI: 10.1080/02773813.2011.562338

Analysis of Lignin Aromatic Structure in Wood Based on the IR Spectrum
journal, October 2012

Non-Destructive Determination of Lignin Syringyl/Guaiacyl Monomeric Composition in Native Wood by Fourier Transform Raman Spectroscopy
journal, February 1998

Interpretive Spectroscopy for Near Infrared
journal, August 1996

A Review of Band Assignments in near Infrared Spectra of Wood and Wood Components
journal, January 2011

  • Schwanninger, Manfred; Rodrigues, José Carlos; Fackler, Karin
  • Journal of Near Infrared Spectroscopy, Vol. 19, Issue 5
  • DOI: 10.1255/jnirs.955

Determination of Eucalyptus Globulus Wood Extractives Content by near Infrared-Based Partial Least Squares Regression Models: Comparison between Extraction Procedures
journal, January 2012

  • Alves, Ana M. M.; Simões, Rita F. S.; Santos, Claudia A.
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  • DOI: 10.1255/jnirs.987

Classification of Lignins from Different Botanical Origins by FT-IR Spectroscopy
journal, January 1991

The Difference of Reactivity between Syringyl Lignin and Guaiacyl Lignin in Alkaline Systems
journal, January 1995

Eucalypts as a biofuel feedstock
journal, November 2011

  • Shepherd, Mervyn; Bartle, John; Lee, David J.
  • Biofuels, Vol. 2, Issue 6
  • DOI: 10.4155/bfs.11.136

Lignin content in natural Populus variants affects sugar release
text, January 2011

  • Studer, Michael Hans-Peter; DeMartini, J. D.; Davis, M. F.
  • National Academy of Sciences
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Raman Spectroscopy for Chemical Analysis
book, January 2000

Rapid determination of syringyl: Guaiacyl ratios using FT-Raman spectroscopy
journal, November 2011

  • Sun, Lan; Varanasi, Patanjali; Yang, Fan
  • Biotechnology and Bioengineering, Vol. 109, Issue 3
  • DOI: 10.1002/bit.24348

Fourier Transform Infrared Spectroscopy
book, January 1992

Estimation of Aromatic Structure Contents in Hardwood Lignins from IR Absorption Spectra
journal, November 2013

Assessment of Lignocellulosic Biomass Using Analytical Spectroscopy: an Evolution to High-Throughput Techniques
journal, July 2013

1064nm dispersive multichannel Raman spectroscopy for the analysis of plant lignin
journal, November 2011

  • Meyer, Matthew W.; Lupoi, Jason S.; Smith, Emily A.
  • Analytica Chimica Acta, Vol. 706, Issue 1
  • DOI: 10.1016/j.aca.2011.08.031

An overview of second generation biofuel technologies
journal, March 2010

Determining the influence of eucalypt lignin composition in paper pulp yield using Py-GC/MS
journal, August 2005

  • del Río, José C.; Gutiérrez, Ana; Hernando, Marina
  • Journal of Analytical and Applied Pyrolysis, Vol. 74, Issue 1-2
  • DOI: 10.1016/j.jaap.2004.10.010

Composition of non-woody plant lignins and cinnamic acids by Py-GC/MS, Py/TMAH and FT-IR
journal, May 2007

  • del Río, José C.; Gutiérrez, Ana; Rodríguez, Isabel M.
  • Journal of Analytical and Applied Pyrolysis, Vol. 79, Issue 1-2
  • DOI: 10.1016/j.jaap.2006.09.003

Evaluation of portable Raman spectrometer with 1064nm excitation for geological and forensic applications
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Development of the partial least squares models for the interpretation of the UV resonance Raman spectra of lignin model compounds
journal, January 2005

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  • Vibrational Spectroscopy, Vol. 37, Issue 1
  • DOI: 10.1016/j.vibspec.2004.08.001

Raman Spectra of Celluloses
book, June 1987

Hydrogen Bonding in Lignin:  A Fourier Transform Infrared Model Compound Study
journal, September 2005

  • Kubo, Satoshi; Kadla, John F.
  • Biomacromolecules, Vol. 6, Issue 5
  • DOI: 10.1021/bm050288q

Identifying Softwoods and Hardwoods by Infrared Spectroscopy
journal, December 1999

  • Barker, Brady; Owen, Noel L.
  • Journal of Chemical Education, Vol. 76, Issue 12
  • DOI: 10.1021/ed076p1706

Theoretical and Raman Spectroscopic Studies of Phenolic Lignin Model Monomers
journal, June 2010

  • Larsen, Kiki L.; Barsberg, Søren
  • The Journal of Physical Chemistry B, Vol. 114, Issue 23
  • DOI: 10.1021/jp1028239

Lignin content in natural Populus variants affects sugar release
journal, March 2011

  • Studer, M. H.; DeMartini, J. D.; Davis, M. F.
  • Proceedings of the National Academy of Sciences, Vol. 108, Issue 15, p. 6300-6305
  • DOI: 10.1073/pnas.1009252108

FT–Raman Investigation of Milled-Wood Lignins: Softwood, Hardwood, and Chemically Modified Black Spruce Lignins
journal, October 2011

  • Agarwal, Umesh P.; McSweeny, James D.; Ralph, Sally A.
  • Journal of Wood Chemistry and Technology, Vol. 31, Issue 4
  • DOI: 10.1080/02773813.2011.562338

Analysis of Lignin Aromatic Structure in Wood Based on the IR Spectrum
journal, October 2012

Non-Destructive Determination of Lignin Syringyl/Guaiacyl Monomeric Composition in Native Wood by Fourier Transform Raman Spectroscopy
journal, February 1998

Interpretive Spectroscopy for Near Infrared
journal, August 1996

Evaluation of plant biomass resources available for replacement of fossil oil
journal, April 2010

Bioenergy from plants and the sustainable yield challenge
journal, July 2008

Cellulosic Biofuels
journal, June 2009

Lignin monomer composition affects Arabidopsis cell-wall degradability after liquid hot water pretreatment
journal, January 2010

  • Li, Xu; Ximenes, Eduardo; Kim, Youngmi
  • Biotechnology for Biofuels, Vol. 3, Issue 1
  • DOI: 10.1186/1754-6834-3-27

A Review of Band Assignments in near Infrared Spectra of Wood and Wood Components
journal, January 2011

  • Schwanninger, Manfred; Rodrigues, José Carlos; Fackler, Karin
  • Journal of Near Infrared Spectroscopy, Vol. 19, Issue 5
  • DOI: 10.1255/jnirs.955

Determination of Eucalyptus Globulus Wood Extractives Content by near Infrared-Based Partial Least Squares Regression Models: Comparison between Extraction Procedures
journal, January 2012

  • Alves, Ana M. M.; Simões, Rita F. S.; Santos, Claudia A.
  • Journal of Near Infrared Spectroscopy, Vol. 20, Issue 2
  • DOI: 10.1255/jnirs.987

Ultra Violet Resonance Raman Spectroscopy in Lignin Analysis: Determination of Characteristic Vibrations of p -Hydroxyphenyl, Guaiacyl, and Syringyl Lignin Structures
journal, January 2003

  • Saariaho, Anna-Maija; Jääskeläinen, Anna-Stiina; Nuopponen, Mari
  • Applied Spectroscopy, Vol. 57, Issue 1
  • DOI: 10.1366/000370203321165214

Characterization of Woody and Herbaceous Biomasses Lignin Composition with 1064 nm Dispersive Multichannel Raman Spectroscopy
journal, August 2012

  • Lupoi, Jason S.; Smith, Emily A.
  • Applied Spectroscopy, Vol. 66, Issue 8
  • DOI: 10.1366/12-06621

Classification of Lignins from Different Botanical Origins by FT-IR Spectroscopy
journal, January 1991

The Difference of Reactivity between Syringyl Lignin and Guaiacyl Lignin in Alkaline Systems
journal, January 1995

Genetic Variation in the Chemical Components of Eucalyptus globulus Wood
journal, July 2011

  • Stackpole, Desmond J.; Vaillancourt, René E.; Alves, Ana
  • G3: Genes|Genomes|Genetics, Vol. 1, Issue 2
  • DOI: 10.1534/g3.111.000372

Eucalypts as a biofuel feedstock
journal, November 2011

  • Shepherd, Mervyn; Bartle, John; Lee, David J.
  • Biofuels, Vol. 2, Issue 6
  • DOI: 10.4155/bfs.11.136
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    Works referencing / citing this record:

    Infrared and Raman spectra of lignin substructures: Coniferyl alcohol, abietin, and coniferyl aldehyde
    journal, April 2019

    • Bock, Peter; Gierlinger, Notburga
    • Journal of Raman Spectroscopy
    • DOI: 10.1002/jrs.5588

    Near-infrared-based models for lignin syringyl/guaiacyl ratio of Eucalyptus benthamii and E. pellita using a streamlined thioacidolysis procedure as the reference method
    journal, April 2019

    • Diniz, Carolina Pinto; Grattapaglia, Dario; Mansfield, Shawn D.
    • Wood Science and Technology, Vol. 53, Issue 3
    • DOI: 10.1007/s00226-019-01090-3

    Advanced spectroscopy-based phenotyping offers a potential solution to the ash dieback epidemic
    journal, November 2018

    Lignocellulosic Biomass: Understanding Recalcitrance and Predicting Hydrolysis
    journal, December 2019

    Prediction of Cell Wall Properties and Response to Deconstruction Using Alkaline Pretreatment in Diverse Maize Genotypes Using Py-MBMS and NIR
    journal, October 2016

    Recent innovations in analytical methods for the qualitative and quantitative assessment of lignin
    journal, September 2015

    • Lupoi, Jason S.; Singh, Seema; Parthasarathi, Ramakrishnan
    • Renewable and Sustainable Energy Reviews, Vol. 49
    • DOI: 10.1016/j.rser.2015.04.091

    Advanced spectroscopy-based phenotyping offers a potential solution to the ash dieback epidemic
    journal, November 2018

    Evaluating Lignocellulosic Biomass, Its Derivatives, and Downstream Products with Raman Spectroscopy
    journal, April 2015

    • Lupoi, Jason S.; Gjersing, Erica; Davis, Mark F.
    • Frontiers in Bioengineering and Biotechnology, Vol. 3
    • DOI: 10.3389/fbioe.2015.00050

    Lignocellulosic Biomass: Understanding Recalcitrance and Predicting Hydrolysis
    journal, December 2019

    Application of Infrared and Raman Spectroscopy for the Identification of Disease Resistant Trees
    journal, January 2016

    Identifying Plant Part Composition of Forest Logging Residue Using Infrared Spectral Data and Linear Discriminant Analysis
    journal, August 2016

    • Acquah, Gifty; Via, Brian; Billor, Nedret
    • Sensors, Vol. 16, Issue 9
    • DOI: 10.3390/s16091375
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