High-throughput Screening of Recalcitrance Variations in Lignocellulosic Biomass: Total Lignin, Lignin Monomers, and Enzymatic Sugar Release

Decker, Stephen R.; Sykes, Robert; Turner, Geoffrey B.; Lupoi, Jason S.; Doepkke, Crissa; Tucker, Melvin P.; Schuster, Logan A.; Mazza, Kimberly; Himmel, Michael E.; Davis, Mark F.; Gjersing, Erica

doi:10.3791/53163

Cited by 17 publications

(14 citation statements)

References 27 publications

(30 reference statements)

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“…For instance, Selig et al developed a high throughput method to determine glucan and xylan content in poplar, pine, wheat stover and pine using a glucose oxidase and a xylose dehydrogenase-based assays instead of HPLC analysis which reduced remarkably the duration of the analysis from 48 to 5-6 h (Selig et al, 2011). Pyrolysis-molecular beam mass spectrometry was used as a high throughput technique to analyse lignin content and structure and polysaccharides content in LB feedstocks (Penning et al, 2014;Decker et al, 2015;Sykes et al, 2015;Harman-Ware et al, 2017). Decker et al (2012) developed a high throughput method to investigate the effect of the starch content in a set of 250 switchgrass variants on the recalcitrance after hydrothermal pre-treatment and enzymatic hydrolysis (5 days).…”

Section: Predicting Enzymatic Hydrolysismentioning

confidence: 99%

Lignocellulosic Biomass: Understanding Recalcitrance and Predicting Hydrolysis

2019

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Lignocellulosic biomass (LB) is an abundant and renewable resource from plants mainly composed of polysaccharides (cellulose and hemicelluloses) and an aromatic polymer (lignin). LB has a high potential as an alternative to fossil resources to produce second-generation biofuels and biosourced chemicals and materials without compromising global food security. One of the major limitations to LB valorisation is its recalcitrance to enzymatic hydrolysis caused by the heterogeneous multi-scale structure of plant cell walls. Factors affecting LB recalcitrance are strongly interconnected and difficult to dissociate. They can be divided into structural factors (cellulose specific surface area, cellulose crystallinity, degree of polymerization, pore size and volume) and chemical factors (composition and content in lignin, hemicelluloses, acetyl groups). Goal of this review is to propose an up-to-date survey of the relative impact of chemical and structural factors on biomass recalcitrance and of the most advanced techniques to evaluate these factors. Also, recent spectral and water-related measurements accurately predicting hydrolysis are presented. Overall, combination of relevant factors and specific measurements gathering simultaneously structural and chemical information should help to develop robust and efficient LB conversion processes into bioproducts.

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Section: Predicting Enzymatic Hydrolysismentioning

confidence: 99%

Lignocellulosic Biomass: Understanding Recalcitrance and Predicting Hydrolysis

2019

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“…Plant material for this study consisted of 2-year-old Salix viminalis shoots from a previously described population, consisting of 291 genetically distinct individuals, collected in the wild in Europe and Russia and planted in a randomized complete block experiment in Pustnäs, Uppsala, Sweden (59°48' N, 17°39' E) [26]. EH sugar yields were previously measured as glucose, xylose, and combined glucose + xylose values using a miniaturized high-throughput pretreatment and saccharification assay [27,28]. A subset of samples from this population (n = 94, encompassing 71 distinct genotypes) was chosen such as to reflect the full range of EH recalcitrance, i.e., sugar release values, with the range of values spanning 0.09-0.45 g/g dry biomass for combined glucose and xylose release.…”

Section: Plant Materialsmentioning

confidence: 99%

Biomass Recalcitrance in Willow Under Two Biological Conversion Paradigms: Enzymatic Hydrolysis and Anaerobic Digestion

et al. 2019

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Biomass recalcitrance, the inherent resistance of plants towards deconstruction, negatively affects the viability of biorefineries. This trait is not only dictated by the properties of the biomass but also by the conversion system used and its interactions with specific features of the biomass. Here, biomass recalcitrance to anaerobic digestion (AD) was assessed using a biomethanation potential (BMP) assay. Plant material (n = 94) was selected from a large population of natural Salix viminalis accessions, previously evaluated for biomass recalcitrance using hydrothermal pretreatment-enzymatic hydrolysis. Correlations between yields from the two biological conversion systems were evaluated, as well as the influence of biomass compositional features, analyzed by pyrolysis-molecular beam mass spectrometry (py-MBMS), and other biomass physical properties on conversion performance. BMP values averaged 198.0 Nml CH 4 /g biomass after 94 days, ranging from 28.6 to 245.9. S lignin and carbohydrate-derived spectral features were positively correlated with performance under both systems, whereas G lignin, pcoumaric acid, and ferulic acid-derived ions were negatively correlated with yields and rates. Most spectral features were more strongly correlated with enzymatic hydrolysis yields compared to methane production. For early-stage methane production and rate, recalcitrance factors were similar compared to enzymatic hydrolysis, with weaker correlations observed at later timepoints. The results suggest that although variation in methane potential was considerably lower than enzymatic hydrolysis yields, a reduced recalcitrance under this system will still be of importance to improve early conversion rates. Spectral features of low methane-producing samples indicate the presence of inhibitory substances, warranting further study.

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“…Populus trichocarpa biomass was grown as outlined in Table 7 and samples were dried and debarked, milled, destarched and extracted with ethanol/water prior to analysis [39]. Mans eld et al [51] were used and integrations were performed using TopSpin 3.6.…”

Section: Biomassmentioning

confidence: 99%

“…Methods that measure the S/G ratio by analyzing pyrolysis products give highly reproducible results; however, the measured S/G ratios do not always compare well with other degradative techniques [29][30][31][32][33][34]. Pyrolysis or thermal degradative methods coupled with chromatographic and/or mass spectrometry techniques can be performed on whole or minimally processed biomass and can be used in high-throughput platforms to analyze lignin content and composition in biomass [3,[35][36][37][38][39]. However, thermal degradation may overestimate the S content as products generated from labile ether linkages are detected whereas condensed linkages (either inherent or produced) may not be incorporated in the analyses, not unlike chemical degradation methods [40,41].…”

Section: Introductionmentioning

confidence: 99%

Comparison of Methodologies Used to Determine Monolignol Ratios in Lignocellulosic Biomass

Happs

Addison

Doeppke

et al. 2020

Preprint

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BackgroundMultiple analytical methods have been developed to determine the ratios of monolignol monomers, particularly the syringyl/guaiacyl (S/G) ratio, of lignin biopolymers in plant cell walls. Chemical degradation methods yield monomers that are either selective of certain linkages, such as thioacidolysis, or induce chemical changes rendering it impossible to distinguish and determine the source of specific monomers, such as nitrobenzene oxidation. NMR methods provide powerful tools used to analyze cell walls for lignin monomeric composition and linkage information. Pyrolysis-mass spectrometry methods are also widely used, particularly as a high-throughput method. However, the different techniques used to analyze lignin monolignol ratios frequently yield different results within particular studies, making it difficult to interpret and compare results, and to obtain meaningful insights relating these measurements to other characteristics of plant cell walls that may impact biomass sustainability and conversion metrics for the production of bio-derived fuels and chemicals.ResultsThe authors compared the S/G monolignol ratios of pine, several genotypes of poplar, and corn stover biomass obtained from thioacidolysis, pyrolysis-molecular beam mass spectrometry (py-MBMS), HSQC liquid-state NMR and solid-state (ss) NMR methodologies. An underutilized approach to deconvolute ssNMR spectra was implemented to derive S/G ratios. The S/G ratios obtained for the samples did not agree across the different methods, but trends were similar with the most agreement among the py-MBMS, HSQC NMR and deconvoluted ssNMR methods. The relationship between monolignol S/G, thioacidolysis yields, and linkage analysis determined by HSQC is also addressed.ConclusionsThis work demonstrates that different methods using chemical, thermal, and nondestructive NMR techniques to determine native monolignol S/G ratios in plant cell walls may yield different results depending on species and linkage abundances. Spectral deconvolution likely applies well to many hardwoods that are S and G dominant, but results may not be reliable for some woody and grassy species for which the lignin composition is more diverse. HSQC may be a better method for analyzing lignin in those species given the wealth of information provided on additional aromatic moieties and bond linkages. Careful consideration is required when choosing a method to measure S/G ratios and the benefits and shortcomings of each method discussed here are summarized.

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High-throughput Screening of Recalcitrance Variations in Lignocellulosic Biomass: Total Lignin, Lignin Monomers, and Enzymatic Sugar Release

Cited by 17 publications

References 27 publications

Lignocellulosic Biomass: Understanding Recalcitrance and Predicting Hydrolysis

Lignocellulosic Biomass: Understanding Recalcitrance and Predicting Hydrolysis

Biomass Recalcitrance in Willow Under Two Biological Conversion Paradigms: Enzymatic Hydrolysis and Anaerobic Digestion

Comparison of Methodologies Used to Determine Monolignol Ratios in Lignocellulosic Biomass

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