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Considering the toxicity of the impurities of synthesized anthraquinone, this study clarified new catalytic compounds for kraft cooking with improved carbohydrate yield and delignification and less mutagenicity, which are important for ensuring the safety of paper products in contact with food. The 2-methylanthraquinone contents of teak ( Tectona grandis ) woods were 0.18-0.21%. Acetone extracts containing 2-methylanthraquinone from Myanmar and Indonesia teak woods as additives improved lignin removal during kraft cooking of eucalyptus wood, which resulted in kappa numbers that were 2.2-6.0 points lower than the absence of additive. Myanmar extracts and 2-methylanthraquinone improved carbohydrate yield in pulps with 1.7-2.2% yield gains. Indonesia extracts contained more deoxylapachol and its isomer than 2-methylanthraquinone. The residual content of 2-methylanthraquinone in the kraft pulp was trace. Although Ames tests showed that the Indonesia and Myanmar extracts were mutagenic to Salmonella typhimurium , 2-methylanthraquinone was not. The kraft pulp obtained with the additives should be safe for food-packaging applications, and the addition of 0.03% 2-methylanthraquinone to kraft cooking saves forest resources and fossil energy in industries requiring increased pulp yield.

To elucidate the chemical linkages between lignin and carbohydrates in ginkgo cell walls, 13 C- 2 H-enriched cell wall-dehydrogenation polymers (CW-DHP) were selectively prepared with cambial tissue from Ginkgo biloba L. by feeding D-glucose-[6- 2 H 2 ], coniferin-[α- 13 C], and phenylalanine ammonia-lyase (PAL) inhibitor. The abundant detection of 13 C and 2 H confirmed that D-glucose-[6- 2 H 2 ] and coniferin-[α- 13 C] were involved in the normal metabolism of ginkgo cambial cells that had been effectively labelled with dual isotopes. In the ginkgo CW-DHP, ketal and ether linkages were formed between the C-α of lignin side chains and carbohydrates, as revealed by solid state CP/MAS 13 C-NMR differential spectroscopy. Furthermore, the DMSO/TBAH ionic liquids system was used to fractionate the ball-milled CW-DHP into three lignin-carbohydrate complex (LCC) fractions: glucan-lignin complex (GL), glucomannan-lignin complex (GML), and xylan-lignin complex (XL). The XRD determination indicated that the cellulose type I of the GL was converted into cellulose type II during the separation process. The molecular weight was in the order of Ac-GL > Ac-GML > XL. The 13 C-NMR and 1 H-NMR differential spectroscopy of 13 C- 2 H-enriched GL fraction indicated that lignin was linked with cellulose C-6 by benzyl ether linkages. It was also found that there were benzyl ether linkages between the lignin side chain C-α and glucomannan C-6 in the 13 C- 2 H-enriched GML fraction. The formation of ketal linkages between the C-α of lignin and xylan was confirmed in the 13 C- 2 H-enriched XL fraction.

A facile and environmentally-friendly strategy for increasing antioxidant activity is a crucial issue for value-added lignin and lignin-carbohydrate complex (LCC) as alternative antioxidants. However, the antioxidant activities of lignin and LCC by the traditional solid-liquid extraction (SLE) methods were restricted by the relatively lower solubility induced from high molecular weight (Mw), and the less functional groups including, phenolic hydroxyl and carboxyl. To improve the antioxidantion of lignin and LCC, lithium chloride/dimethyl sulfoxide (LiCl/DMSO) solvent fractionation (LDSF) was conducted to increase the functional groups and reduce Mw, in which LiCl/DMSO acted triple roles as solvent, acid, and metal chloride catalyst for the depolymerization reaction synchronously. The β-O-4' linkages were cleaved to release the phenolic hydroxyl, resulting in decreasing Mw; the hydroxyl of the side-chain of lignin was oxidized into carboxyl. Thus, the lignin (LD-RL) and LCC (LD-LCC) samples from LDSF had a higher syringyl (S)/guaiacyl (G) ratio, phenolic hydroxyl, and carboxyl contents, but less Mw than control groups from SLE. Consequently, they presented more excellent scavenging rates toward DPPH and ABTS radicals, up to 90%. This work provided panoramic perspectives and basics of the green and convenient approach to isolate and modify lignin and LCC for great antioxidantion with LDSF., (Copyright © 2021. Published by Elsevier B.V.)

Since the pandemic outbreak of Covid-19 in December 2019, several lateral flow assay (LFA) devices were developed to enable the constant monitoring of regional and global infection processes. Additionally, innumerable lateral flow test devices are frequently used for determination of different clinical parameters, food safety, and environmental factors. Since common LFAs rely on non-biodegradable nitrocellulose membranes, we focused on their replacement by cellulose-composed, biodegradable papers. We report the development of cellulose paper-based lateral flow immunoassays using a carbohydrate-binding module-fused to detection antibodies. Studies regarding the protein binding capacity and potential protein wash-off effects on cellulose paper demonstrated a 2.7-fold protein binding capacity of CBM-fused antibody fragments compared to the sole antibody fragment. Furthermore, this strategy improved the spatial retention of CBM-fused detection antibodies to the test area, which resulted in an enhanced sensitivity and improved overall LFA-performance compared to the naked detection antibody. CBM-assisted antibodies were validated by implementation into two model lateral flow test devices (pregnancy detection and the detection of SARS-CoV-2 specific antibodies). The CBM-assisted pregnancy LFA demonstrated sensitive detection of human gonadotropin (hCG) in synthetic urine and the CBM-assisted Covid-19 antibody LFA was able to detect SARS-CoV-2 specific antibodies present in serum. Our findings pave the way to the more frequent use of cellulose-based papers instead of nitrocellulose in LFA devices and thus potentially improve the sustainability in the field of POC diagnostics.

An individual nanoparticle-based plasmonic nanotechnology was used for real-time monitoring of lectin-sugar interactions, which could be designed as novel plasmonic nanobiosensors for the detection of trace concanavalin A (ConA) with high sensitivity and selectivity. The localized surface plasmon resonance (LSPR) spectra of Au@Ag nanocubes (NCs) are linearly shifted to a long wavelength with an increasing concentration of ConA. In fact, each Au@Ag NC can act as a nanobiosensor for the quantified detection of trace ConA, which enables the miniaturization of the biosensor system to nanoscale. Furthermore, the results demonstrated the perfect biosensing ability with the dual channel of dark-field microscopy images and LSPR spectra. We expect that this nanobiosensor system can provide an alternative important method for monitoring the specific binding of lectin-sugar at a single nanoparticle surface.

An efficient one-pot approach for the production of levulinate ester from renewable carbohydrates is demonstrated over heteropolyanion-based ionic liquid (IL-POM) catalysts with alcohols as the promoters and solvents. The relationships between the structure, acidic strength, and solubility of the IL-POM in methanol and the catalytic performance were studied intensively. A cellulose conversion of 100 % could be achieved with a 71.4 % yield of methyl levulinate over the catalyst [PyPS] 3 PW 12 O 40 [PyPS=1-(3-sulfopropyl)pyridinium] at 150 °C for 5 h. This high efficiency is ascribed to the reasonably high activity of the ionic liquid (IL) catalyst and reaction coupling with rapid in situ esterification of the generated levulinic acid with the alcohol promoter, which allows the insolubility of cellulose encountered in biomass conversion to be overcome. Furthermore, the present process exhibits high feedstock adaptability for typical carbohydrates and handy catalyst recovery by a simple self-separation procedure through temperature control., (© 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Acidification has been commercialized for producing kraft lignin from black liquor of kraft pulping process. This work intended to evaluate the effectiveness of acidification in extracting lignocelluloses from the spent liquor of neutral sulfite semichemical pulping (NSSC) process and from prehydrolysis liquor (PHL) of kraft-based dissolving pulp production process. The results showed that the NSSC and PHL spent liquors had some lignin-carbohydrate complexes (LCC), and that the square weighted counts of particles with a chord length of 50-150μm in the spent liquors were significantly increased as pH dropped to 1.5. Interestingly, the acidification reduced the lignosulfonate/lignin content of NSSC and PHL by 13% or 20%, while dropped their oligosugars content by 75% and 38%, respectively. On a dry basis, the precipitates had more carbon, hydrogen and a high heating value of 18-22MJ/kg, but less oxygen, than spent liquors. The precipitates of PHL could be used as fuel., (Copyright © 2016 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

In this study, mild acid hydrolysis using γ-valerolactone (GVL)/water system integrated with enzymatic hydrolysis was carried out for the enhancement of enzymatic saccharification efficiency. The quantitative analysis of soluble carbohydrates and structural characterizations of solid residues were conducted. Results showed that the soluble carbohydrates in the water-phase were mainly composed of monomers and oligomers from xylose and glucose, while the contents of which were depended on the ratio of GVL to water. Moreover, the inhibitors were hardly detected due to the moderate pretreatment severity. Compared with the untreated feedstock, the yields of enzymatic hydrolysis from pretreated samples increased by two-fold with the mixture of 80/20 GVL/H2O. Combined with the amount of glucose (14.6%) dissolved in the water-phase, over 92.6% of glucose in cotton stalk was released and recovered. Based on the comprehensive analysis, treatment with GVL/H2O system provided us a more effective approach for sugar production from biomass., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

A novel fluorescence-based immunochromatographic assay (ICA) for rapid detecting 4(5)-methylimidazole (4-MI) is presented in this study. In our work, the conjugates of fluorescent microspheres (FMs) and 4-MI monoclonal antibody were used as probe for ICA. Under optimal conditions, a standard curve of ICA-based detection of 4-MI was developed, linear detection ranged from 0.50 to 32.0 mg/L. The cross-reactivities were observed less than 3.93% by detecting 6 selected structural analogues of 4-MI. The recoveries of 4-MI in caramels detection were ranged from 82.85% to 102.31%, with the coefficient of variation (n = 3) below 9.06%. Quantitative comparison of the established fluorescence-based ICA with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) analysis of real caramel colour samples indicated a good correlation among the methods. Therefore, our developed fluorescence-based ICA method shows great potential for simple, rapid, sensitive, and cost-effective quantitative detection of 4-MI in food safety control., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Prehydrolysis of wood biomass prior to kraft cooking provides a stream containing hemicellulose-derived saccharides (HDSs) but also undesired non-saccharide compounds (NSCs) that were resulted from lignin depolymerization and carbohydrate degradation. In this study, a combined process consisting of lime treatment, resin adsorption, and gel filtration was developed to separate HDSs from NSCs. The macro-lignin impurities that accounted for 32.2% of NSCs were removed by lime treatment at 1.2% dosage with negligible HDSs loss. The majority of NSCs, lignin-derived phenolics, were eliminated by mixed bed ion exchange resin, elevating NSCs removal to 94.0%. The remaining NSCs, furfural and hydroxymethylfurfural, were excluded from HDSs by gel filtration. Chemical composition analysis showed that xylooligosaccharides (XOS) with the degree of depolymerization from 2 to 6 accounted for 28% of the total purified HDSs., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Saccharides and lignin components in prehydrolysis liquor (PHL) from kraft-based dissolving pulp production was characterized after being fractionated using membrane filtration. The results showed that the membrane filtration provided a method for organics fractionation with considerable recovery rate, but exhibited some disadvantages. Besides the limited ability in purifying oligosaccharides (OS) due to the overlaps of molecular weight distribution with lignin components, the membrane filtration could not improve the homogeneity of OS as indicated by the analysis of chemical compositions and the degree of polymerization (DP), which may be ascribed to the linear conformation of OS. The characterization of lignin components indicated a great potential for polymer industry because of the remarkable content of phenolic hydroxyl groups (PhOH), especially for low molecular weight (LMW) fraction. It was concluded the organics in PHL provided streams of value-added chemicals. However, the practical significance thereof can be realized and maximized only when they are successfully and completely fractionated., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Three strategies were presented to achieve high solids loading while maximizing carbohydrate conversion, which are fed-batch, splitting/thickening, and clarifier processes. Enzymatic hydrolysis was performed at water insoluble solids (WIS) of 15% using washed dilute-acid pretreated corn stover. The carbohydrate concentration increased from 31.8 to 99.3g/L when the insoluble solids content increased from 5% to 15% WIS, while the final carbohydrate conversion was decreased from 78.4% to 73.2%. For the fed-batch process, a carbohydrate conversion efficiency of 76.8% was achieved when solid was split into 60:20:20 ratio, with all enzymes added first. For the splitting/thickening process, a carbohydrate conversion of 76.5% was realized when the filtrate was recycled to simulate a steady-state process. Lastly, the clarifier process was evaluated and the highest carbohydrate conversion of 81.4% was achieved. All of these results suggests the possibility of enzymatic hydrolysis at high solids to make the overall conversion cost-competitive., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Acetic acid ethanol-based organosolv pretreatment of sugar cane bagasse was performed to enhance enzymatic hydrolysis. The effect of different parameters (including temperature, reaction time, solvent concentration, and acid catalyst dose) on pretreatment prehydrolyzate and subsequent enzymatic digestibility was determined. During the pretreatment process, 11.83 g of xylose based on 100 g of raw material could be obtained. After the ethanol-based pretreatment, the enzymatic hydrolysis was enhanced and the highest glucose yield of 40.99 g based on 100 g of raw material could be obtained, representing 93.8% of glucose in sugar cane bagasse. The maximum total sugar yields occurred at 190 °C, 45 min, 60:40 ethanol/water, and 5% dosage of acetic acid, reaching 58.36 g (including 17.69 g of xylose and 40.67 g of glucose) based on 100 g of raw material, representing 85.4% of total sugars in raw material. Furthermore, characterization of the pretreated sugar cane bagasse using X-ray diffraction and scanning electron microscopy analyses were also developed. The results suggested that ethanol-based organosolv pretreatment could enhance enzymatic digestibilities because of the delignification and removal of xylan.

The specific elimination of lignin derivatives from wood hydrolysate without sugar loss has great practical significance to biorefinery and bioenergy. In the present study, a process consisting of calcium hydroxide and anion exchange resin treatments was developed for the purpose of selective removal of lignin from wood prehydrolysis liquor (PHL). Particular emphasis was made on the ionization of phenolic lignin, and the subsequent binding to metallic salts. It was observed that phenolic hydroxyl groups (PhOH) in lignin played an important role in lignin removal. The results showed that up to 95.2% lignin was removed from PHL with 78.8% sugar recovery. This suggested that the proposed process is highly specific to lignin, and therefore can be envisaged as a great contribution to wood-sugar production or bioenergy conversion., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

InCl3, a water-compatible Lewis acid, was used for the conversion of microcrystalline cellulose to produce 5-hydroxymethylfurfural (HMF) in a H2O/THF biphasic system. Addition of NaCl increased the HMF yield significantly but suppressed the levulinic acid (LA) formation. The HMF yield of 39.7% was obtained in 2h at 200°C in the NaCl-H2O/THF catalytic system catalyzed by InCl3. The catalytic system also showed effectiveness to convert other carbohydrates to HMF, including glucose, fructose, sucrose, starch, which demonstrated great potential towards different feedstocks., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

A simultaneous analysis of methylimidazoles, reducing sugars, and 5-hydroxymethyl-2-furaldehyde in the Maillard reaction was improved by use of an amino trap column. Analysis was carried out by using high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) coupled with an amino trap column. The amino trap column was a useful tool to improve the separation of methylimidazoles, reducing sugars, and 5-hydroxymethyl-2-furaldehyde. This technique is useful for simultaneous analysis of methylimidazoles, reducing sugars, and 5-hydroxymethyl-2-furaldehyde in risk assessment for dairy products., (Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.)

A novel interface that enables high-performance anion-exchange chromatography (HPAEC) to be coupled with electrospray ionization (ESI) mass spectrometry (MS) is reported. A sheath liquid consisting of 50mM NH4Ac in isopropanol with 0.05% acetic acid, infused at a flow rate of 3μL/min at the tip of the electrospray probe, requires less ESI source cleaning and promotes efficient ionization of mono- and di-carbohydrates. The results suggest that use of a sheath liquid interface rather than a T-joint allows volatile ammonium salts to replace non-volatile metal salts as modifiers for improving sugar ESI signals. The efficient ionization of mono- and di-carbohydrates in the ESI source is affected by the sheath liquid properties such as buffer concentration and type of organic solvent. HPAEC-ESI-MS was used for the analysis of monocarbohydrates in pectins, particularly co-eluted sugars, and the performance was evaluated. Addition of a make-up solution through the sheath liquid interface proved to be an efficient tool for enhancing the intensities of sugars analyzed using HPAEC-ESI-MS., (Copyright © 2014 Elsevier B.V. All rights reserved.)

The roles of brassinosteroids (BRs) in vasculature development have been implicated based on an analysis of Arabidopsis BR mutants and suspension cells of Zinnia elegans. However, the effects of BRs in vascular development of a woody species have not been demonstrated. In this study, 24-epi brassinolide (BL) was applied to the vascular cambium of a vertical stem of a 2-year-old Liriodendron, and the resulting chemical and anatomical phenotypes were characterized to uncover the roles of BRs in secondary xylem formation of a woody species. The growth in xylary cells was clearly promoted when treated with BL. Statistical analysis indicated that the length of both types of xylary cells (fiber and vessel elements) increased significantly after BL application. Histochemical analysis demonstrated that BL-induced growth promotion involved the acceleration of cell division and cell elongation. Histochemical and expression analysis of several lignin biosynthetic genes indicated that most genes in the phenylpropanoid pathway were significantly down-regulated in BL-treated stems compared to that in control stems. Chemical analysis of secondary xylem demonstrated that BL treatment induced significant modification in the cell wall carbohydrates, including biosynthesis of hemicellulose and cellulose. Lignocellulose crystallinity decreased significantly, and the hemicellulose composition changed with significant increases in galactan and arabinan. Thus, BL has regulatory roles in the biosynthesis and modification of secondary cell wall components and cell wall assembly during secondary xylem development in woody plants., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

The present work investigated the effects of subcritical CO2 pretreatment of sugarcane bagasse at different CO2 pressure, pretreatment time, and temperature with relative high-solid concentration (15% w/v) to the composition of prehydrolyzate and the enzymatic hydrolysis. The results indicated that the maximum xylose yields in prehydrolyzate liquid were 15.78 g (combined 3.16 g xylose and 12.62 g xylo-oligosaccharides per 100g raw material). Due to the effective removal of hemicellulose, the maximum glucose yield in enzyme hydrolyzate reached 37.99 g per 100g raw material, representing 91.87% of glucose in the sugarcane bagasse. The maximal total sugars yield (combined xylose and glucose both in prehydrolyzate and enzymatic hydrolyzate) were 52.95 g based on 100g raw material. These results indicated that subcritical CO2 pretreatment can effectively improve the enzymatic hydrolysis, so it could be successfully applied to sugarcane bagasse., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Lignocellulosic biomass can be utilized to produce promising biofuels. In this study, liquid hot water pretreatments were performed to break the intricate structure of sugarcane bagasse, which resists the enzyme accessibility to cellulose. The effects of temperatures and times on the hemicellulose degradation (including the yields of pentoses and hexoses, the proportion of monomers and oligosaccharides, as well as limited inhibitors) and cellulose enzymatic digestibility were evaluated. The results indicated that the maximum xylose yields (combined 3.85 g xylose and 13.21 g xylo-oligosaccharides per 100 g raw material) in prehydrolyzate liquid were obtained at 180 °C and 30 min. Due to the effective removal of hemicellulose, the maximum glucose yield in enzyme hydrolyzate reached 37.27 g per 100 g raw material, representing 90.13% of glucose in the sugarcane bagasse. The maximal total sugars yield (combined prehydrolyzate and enzymatic hydrolyzate) were 53.65 g based on 100 g raw material., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Rice straw is one of the most abundant agricultural residues in China. It is considered as a promising raw material for bioethanol production. In this work, rice straw was pretreated by sodium sulfite-formaldehyde (SF) for improving enzymatic saccharification. The SF pretreatment, using proven technology and industrialized equipment, showed efficient delignification selectivity and high carbohydrates retention in pretreated solid. The highest sugar yields of 79.0%, 88.8% and 71.1% for total sugar, glucan and xylan, respectively were obtained at an enzyme loading of 40 FPU/g-substrate after the raw material pretreated with 12% sodium sulfite at 160°C. About 75% of lignin was dissolved in pretreatment spent liquor and 78% of silica was retained in the residue of enzymatic hydrolysis. The results proved sulfite-formaldehyde as a promising pretreatment for the production of bioethanol as well as potential high value added by-products of silica nanoparticles and lignosulfonate., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

The effects of sodium carbonate (Na(2)CO(3)) pretreatment on the chemical compositions and enzymatic saccharification of rice straw were investigated. The enzymatic digestibility of rice straw is enhanced after pretreatment since pretreated solids show significant delignification with high sugar availability. During pretreatment, an increasing temperature and Na(2)CO(3) charge leads to enhanced delignification, whereas an increased degradation of polysaccharides as well, of which xylan acts more susceptible than glucan. The sugar recovery of enzymatic hydrolysis goes up rapidly with the total titratable alkali (TTA) increasing from 0% to 8%, and then it reaches a plateau. The highest sugar recovery of rice straw after pretreatment, 71.7%, 73.2%, and 76.1% for total sugar, glucan, and xylan, respectively, is obtained at 140°C, TTA 8% and cellulase loading of 20 FPU/g-cellulose. In this condition, the corresponding delignification ratio of pretreated solid is 41.8%, while 95% of glucan and 76% of xylan are conserved., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Dilute sulfuric acid was used to pretreat eucalyptus chips prior to enzymatic hydrolysis. After both pretreatment and enzymatic hydrolysis processes. Attention is paid to sugar recovery. The maximum total sugars yield (combined xylose and glucose, 47.69g/100g raw material, representing 82% of total sugars in the eucalyptus biomass) was obtained at 160°C, 0.75% acid concentration and 10min residence time, which is consider to be the best reasonable conditions for the dilute acid pretreatment of eucalyptus, corresponding concentrations of acetic acid, HMF, and furfural in the prehydrolysate were about 2.01g/L, 0.13g/L and 1.37g/L, respectively. Under this optimal pretreatment condition, the acid-insoluble lignin recovery in the insoluble solid resulting from enzymatic hydrolysis, was 22.7g/100g raw material, representing 80% of acid-insoluble lignin in the eucalyptus biomass., (Copyright © 2012 Elsevier Ltd. All rights reserved.)

Hydrothermal pretreatment was performed on the leaves and internodes portions of Alamo switchgrass, Panicum virgatum L., to enhance the digestibility of cellulose towards cellulase. It was observed that extractives free leaves portion provided 18.1% lower pretreatment gravimetrical yield and 33.8% greater cellulose-to-glucose yield than internodes portion. The degree of polymerization (DP) and ultrastructure of cellulose were determined by gel-permeation chromatography and solid-state cross polarization/magic angle spinning (13)C NMR experiments. The results suggested that hydrothermal pretreatment hydrolyzed amorphous cellulose and yielded a product enriched in paracrystalline cellulose. Furthermore, the DP of cellulose was reduced to one third of the origin value after hydrothermal pretreatment. The resulting biomass after pretreatment for leaves and internodes has similar cellulose ultrastructure and chemical profiles. The results of the enzymatic hydrolysis studies of cellulose suggest that the reduced DP of cellulose of pretreated switchgrass was an important factor influencing the enhanced digestibility of pretreated switchgrass., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

A quantitative approach to characterize lignin-carbohydrate complex (LCC) linkages using a combination of quantitative ¹³C NMR and HSQC 2D NMR techniques has been developed. Crude milled wood lignin (MWLc), LCC extracted from MWLc with acetic acid (LCC-AcOH) and cellulolytic enzyme lignin (CEL) preparations were isolated from loblolly pine (Pinus taeda) and white birch (Betula pendula) woods and characterized using this methodology on a routine 300 MHz NMR spectrometer and on a 950 MHz spectrometer equipped with a cryogenic probe. Structural variations in the pine and birch LCC preparations of different types (MWL, CEL and LCC-AcOH) were elucidated. The use of the high field NMR spectrometer equipped with the cryogenic probe resulted in a remarkable improvement in the resolution of the LCC signals and, therefore, is of primary importance for an accurate quantification of LCC linkages. The preparations investigated showed the presence of different amounts of benzyl ether, γ-ester and phenyl glycoside LCC bonds. Benzyl ester moieties were not detected. Pine LCC-AcOH and birch MWLc preparations were preferable for the analysis of phenyl glycoside and ester LCC linkages in pine and birch, correspondingly, whereas CEL preparations were the best to study benzyl ether LCC structures. The data obtained indicate that pinewood contains higher amounts of benzyl ether LCC linkages, but lower amounts of phenyl glycoside and γ-ester LCC moieties as compared to birch wood.

Aqueous dilute acid pretreatments of corncob were conducted using cylindrical pressure vessels in an oil bath. Pretreatments were conducted in a temperature range of 160-190 °C with acid-solution-to-solid-corncob ratio of 2. The acid concentration (v/v) in the pretreatment solution was varied from 0% to 0.7%, depending on temperature. This gives acid charge on ovendry-weight corncob of 0-2.58%. It was found that optimal pretreatment temperature is between 160 and 170 °C based on total xylose and glucose yields and thermal energy consumption in pretreatment. At 170 °C and acid charge of 2.2% on cob, total glucose yield and xylose recovery were 97% and 75%, respectively, which resulted in an overall monomeric sugar recovery of about 88%. Xylose concentration in the hydrolysate was about 12%, with xylose-to-acetic-acid ratio of 8 and to furan (furfural and hydroxymethylfurfural) of about 15.

Under the current energy scenario, the development of alternatives to fossil fuels, like bioethanol from lignocellulosic materials, is highly relevant. Therefore it is important to search and study new raw materials and to optimize the different steps that lead to bioethanol production. In this work, acid diluted pretreatment was optimized considering the release of sugars. Under the optimal conditions, the reducing sugars yield was of 293.4mg/g of dry biomass in liquid fraction. The tested pretreated samples of Pterospartum tridentatum that presented a higher glucose yield in enzymatic saccharification where those that were subject to a pretreatment at 180°C for 75min with 2.75% (w/w) of sulfuric acid when using a biomass/liquid ratio of 2.25g/10mL leading to a maximum yield of glucose that was 92% of the theoretical maximum. From the fermentation of filtrates it was possible to obtain a maximum ethanol yield of 0.26g ethanol/g total sugars, without previous detoxification., (Copyright © 2010. Published by Elsevier Ltd.)

The focus of this work was to determine the utility of (1)H NMR spectroscopy in the quantification of sugars resulting from the solubilization of hemicelluloses during the autohydrolysis of hardwoods and the use of this technique to evaluate the kinetics of this process over a range of temperatures and times. Yields of residual xylan, xylooligomers, xylose, glucose, and the degraded products of sugars, i.e., furfural and HMF (5-hydroxymethyl furfural), were determined. The monosaccharide and oligomer contents were quantified with a recently developed high resolution (1)H NMR spectroscopic analysis. This method provided precise measurement of the residual xylan and cellulose remaining in the extracted wood samples and xylose and glucose in the hydrolyzates. NMR was found to exhibit good repeatability and provided carbohydrate compositional results comparable to published methods for sugar maple and aspen woods.

Stage-specific analyses of starch and 18 sugars, including pentoses, hexoses, disaccharides, trisaccharides, oligosaccharides and sugar alcohols, were made throughout seed development for zygotic embryo and female gametophyte (FG) tissues of loblolly pine (Pinus taeda L.). Tissue was most often analyzed in triplicate from two open-pollinated families grown in different locations and sampled in different years. Carbohydrates were analyzed by enzymatic assay, high performance liquid chromatography or gas chromatography/mass spectrometry. For all carbohydrates quantified, peak concentrations were higher in embryo tissue than in FG tissue. Significant changes in starch and sugar concentrations occurred over time, with both seed collections showing similar trends in temporal changes. Although concentrations were not always similar, embryo and FG tissues generally showed similar patterns of change in starch and sugar concentrations over time. Total starch concentration was highest during early seed development and decreased as development progressed. The major sugars contributing to osmotic potential during early seed development were D-pinitol, sucrose, fructose and glucose. During mid-seed development, D-pinitol, sucrose, fructose, glucose, melibiose and raffinose provided major contributions to the osmotic environment. During late seed development, sucrose, raffinose, melibiose, stachyose and fructose were the major contributors to osmotic potential. These data suggest stage-specific media composition for each step in the somatic embryogenesis protocol.

Changes in carbohydrate components and crystalline structure of hemp bast fibers during organosolv pulping were investigated by X-ray diffractometry, FT-IR spectroscopy and high performance liquid chromatography (HPLC). The reasons for defibrillation and beating problems with organosolv hemp bast fiber pulp were investigated with reference to these properties of pulp samples. Hemp bast fibers and organosolv pulp samples had low hemicellulose contents and high cellulose contents. It was found that the disorder parameter of cellulose in hemp bast fibers was very low, when crystalline cellulose ratio was high and the crystalline structure of cellulose in hemp bast fibers was very stable. These properties affected defibrillation and beating of organosolv hemp bast fibers pulp negatively.

An efficient method for determining the carbohydrate composition of extractive-free delignified wood and pulp is described here. The polysaccharides in the sample are first hydrolyzed using a mixture of commercially available preparations of cellulase and hemicellulase. The reducing saccharides in the hydrolysate thus obtained are subsequently derivatized with 4-aminobenzoic acid ethyl ester and thereafter quantitated by capillary zone electrophoresis (CZE) in an alkaline borate buffer with monitoring of the absorption at 306 nm. All reducing sugars (i.e., neutral monosaccharides and uronic acids) which occur as structural elements in the polysaccharides of wood and pulp can be quantitated in a single such analytical run, which can also determine the contents of 4-deoxy-beta-L-threo-hex-4-enopyranosyluronic acid (HexA) residues present in pulps obtained from alkaline processes. CZE analyses were performed using linear regression of standard curves over a concentration range spanning approximately three orders of magnitude. Carbohydrate constituents constituting approximately 0.1% of the dry mass of the sample could be quantitated. The overall precision of this analytical procedure--involving enzymatic hydrolysis, derivatization and CZE--was good (RSD=2.2-7.5%), especially considering the heterogeneity of the wood and pulp samples. The total yield of carbohydrates (93-97%) obtained employing the procedure developed here was consistently higher than that obtained upon applying the traditional procedure for carbohydrate analysis (85-93%) (involving acid hydrolysis and gas chromatographic analysis) to the same pulps. The trisaccharide HexA-xylobiose was the only HexA-containing saccharide detected using the conditions for enzymatic hydrolysis developed here (i.e., 30 h incubation at pH 4 and 40 degrees C); whereas mixtures of HexA-xylobiose and HexA-xylotriose were obtained when the incubation was performed at pH 5 or 6.