Fractionation and characterization of lignin carbohydrate complexes (LCCs) of Eucalyptus globulus in residues left after MWL isolation. Part I: Analyses of hemicellulose-lignin fraction (HC-L)

Holzforschung ◽  
2012 ◽  
Vol 66 (4) ◽  
Author(s):  
Yasuyuki Miyagawa ◽  
Ooki Takemoto ◽  
Toshiyuki Takano ◽  
Hiroshi Kamitakahara ◽  
Fumiaki Nakatsubo

Abstract The residual wood meal left after milled wood lignin (MWL) isolation (MWR) was extracted with the cellulose solvent lithium chloride/N,N-dimethylacetamide (LiCl/DMAc) to obtain a soluble fraction (C-L) and an insoluble fraction (C-L-residue). The C-L-residue was further extracted with the hemicellulose solvent 3 M NaOH to give a soluble fraction named hemicellulose-lignin fraction (HC-L) with 21.3% yield based on MWR. It was found that HC-L was composed of xylan, cellulose and lignin with abundant S-type β-O-4 substructures. HC-L lignin was bonded to HC-L cellulose or HC-L hemicelluloses or both. The method, which comprised acetylation for hardwood xylan (by acetic anhydride/pyridine/formamide) and extraction with chloroform, was found to be effective for selective xylan acetate fractionation. HC-L was further fractionated by the same method and subsequent deacetylation to give a xylan-lignin fraction (X-L) in 11.3% yield based on HC-L. X-L was composed mainly of xylan and lignin with abundant S-type β-O-4 substructures, and bonded to X-L xylan. X-L is considered as a promising fraction for elucidation of the structure of lignin-carbohydrate linkages.

Holzforschung ◽  
2006 ◽  
Vol 60 (6) ◽  
pp. 653-658 ◽  
Author(s):  
Hiroyuki Furuno ◽  
Toshiyuki Takano ◽  
Shuichi Hirosawa ◽  
Hiroshi Kamitakahara ◽  
Fumiaki Nakatsubo

Abstract The residual wood meal left after extraction of milled wood lignin (MWL) was extracted with lithium chloride/N,N-dimethylacetamide, which is a well-known cellulose solvent, to afford a soluble fraction (cellulose-lignin fraction; CL) in 36.7% yield. The UV elution curve of CL acetate has the same profile as its refractive index (RI) elution curve. After partial degradation of CL by cellulase, the UV elution curve of CL acetate shifted to the low-molecular-mass region in a similar fashion as its RI elution curve. These results indicate that the lignin in CL (CL lignin) is chemically bonded to cellulose. On the other hand, half of the CL lignin was removed by xylanase treatment. It was concluded that approximately half of the CL lignin existed as a lignin-cellulose-xylan complex.


Holzforschung ◽  
2013 ◽  
Vol 67 (6) ◽  
pp. 629-642 ◽  
Author(s):  
Yasuyuki Miyagawa ◽  
Hiroshi Kamitakahara ◽  
Toshiyuki Takano

Abstract The residual wood meal left after milled wood lignin (MWL) isolation [milled wood residue (MWR)] of 5-year-old Eucalyptus globulus was fractionated to afford a xylan-lignin fraction (X-L) in 2.9% yield (based on MWR) by the method reported previously. X-L was further fractionated with the lignin solvent 1,4-dioxane/water (9:1, v/v) to give a soluble fraction (XL-F1; 24.0%) and an insoluble fraction (XL-F1-residue; 74.6%; both yields based on X-L). XL-F1-residue was further extracted with the good xylan solvent dimethyl sulfoxide and the soluble fraction was termed XL-F2 (43.0%; based on the XL-F1-residue). XL-F1 was mainly composed of lignin with a small amount of xylan and it is similar to purified MWL, whereas XL-F2 was mainly composed of xylan with some amount of lignin and it is similar to a fraction that was prepared by the extraction of crude MWL with acetic acid [lignin-carbohydrate complex (LCC)-AcOH]. The two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance spectra of XL-F1 and XL-F2 were interpreted that the former has α-ether-type lignin-carbohydrate (LC) linkages and the latter might have LC linkages of the phenyl glycoside type, which are different from those in LCC-AcOH.


1980 ◽  
Vol 58 (7) ◽  
pp. 669-676 ◽  
Author(s):  
Jairo H. Lora ◽  
Morris Wayman

In order to obtain further understanding of the nature of lignin reactions during autocatalysed hydrolysis (autohydrolysis) of wood, milled wood lignin (MWL) was isolated from aspen (Populus tremuloides) and treated under autohydrolysis conditions. By this means reactions of the lignin itself could be distinguished from those taking place between lignin and the carbohydrate or other components of the wood. The material after the reaction was separated into a dioxane insoluble fraction (DI), a dioxane soluble but ether insoluble fraction (DSEI), and an ether soluble fraction (ES). Studies were carried out on the DI and DSEI fractions; no direct study was made of the small ES fraction.The formation of DI material increased linearly during the first 7.5 min at 170 °C and then levelled off. At the same time DSEI decreased and then levelled off. Gel permeation chromatography of the DSEI fraction suggested that during autohydrolysis there is an initial generation of low molecular weight fragments which recombine to form first a high molecular weight soluble fraction and from this the insoluble product. The DSEI fraction contained increased conjugated and unconjugated keto groups. Carboxylic acids were also detected; they have been attributed to the reincorporation of low molecular weight aromatic acids generated by the hydrolysis of the corresponding esters. The dioxane insoluble (DI) fraction had fewer unconjugated keto groups than the DSEI fraction, indicating that these groups participated in the condensation reactions leading to the formation of insoluble material. These probably involve position 6 of the aromatic ring.


2019 ◽  
Vol 49 (6) ◽  
Author(s):  
Claudine Garcia Chaves da Costa ◽  
Marielle Maria de Oliveira Paula ◽  
Armando Abel Massingue ◽  
Robledo de Almeida Torres Filho ◽  
Eduardo Mendes Ramos ◽  
...  

ABSTRACT: This study aimed to investigate the extraction and characterization of protein concentrates from pig by-products (heart, liver and kidneys) using the pH-shifting technique. From the solubility profiles (pH 2 to 12), the protein extraction was performed at alkaline pH (10.0 to 11.5), obtaining two fractions: soluble (SC) and insoluble (IC). Higher protein content (71 to 77%) and extractability (214 to 459 mg/g) were observed in heart and liver concentrates; whereas, for water holding capacity (WHC) the highest values (4.20 to 4.54 g water/g protein) were for the heart (SC) and kidney (SC and IC) concentrates. All concentrates had high emulsion stability and higher WHC than commercial protein extenders (whey and soybean). The concentrates obtained from the soluble fraction were redder (higher a* values and lower h values) and darker (lower L* values) than insoluble fraction, especially heart and liver concentrates. Use of concentrates in sausage production slightly altered the color chroma (C*) of samples. It was concluded that the pig by-products protein concentrates had great potential of use as extenders in sausage production.


1975 ◽  
Vol 145 (2) ◽  
pp. 287-297 ◽  
Author(s):  
G Francis ◽  
J Thomas

1. The contents of the fibrous proteins collagen and elastin in the pleural and parenchymal regions of bovine lungs were determined. The collagen content was approx. 70% (g/100g of salt-extracted defatted powder) in each tissue, and the elastin content was 28% in pleura and 13.5% in parenchyma. 2. Purification of the insoluble collagen from the pleura and parenchyma of bovine lungs by various methods was attempted. The collagen fractions isolated after incubation of the pulmonary tissues with the proteolytic enzymes collagenase (“collagenase-soluble” fraction) or pancreatic elastase (“elastase-insoluble” fraction) each contained approx. 87% of the total collagen initially present. 3. Both collagen fractions were chemically analysed for their amino acid and carbohydrate contents and were found to be similar to those of the intact interstitial collagens isolated from skin, bone and tendon. 4. The contents of the two aldimine cross-linking compounds, dehydrohydroxylysinonorleucine and dehydrodihydroxylysinonorleucine, were determined in the bovine pulmonary collagen fractions, and were found to decrease with increasing age of the animals, and were similar to the values found in intact collagens from bone and tendon.


2021 ◽  
Vol 16 (5) ◽  
pp. 1934578X2110233
Author(s):  
Masahiro Saiki ◽  
Naomichi Takemoto ◽  
Maki Nagata ◽  
Masako Matsumoto ◽  
Yhiya Amen ◽  
...  

In recent years, entomophagy has attracted increased attention, as it was recommended as a potential source of food by the Food and Agriculture Organization of the United Nations. In Japan, Oxya yezoensisis one of the most widely eaten insect species, but studies of its functionality as a food are limited. In this study, we reported the optimal characterization of the total phenolic compounds in methanolic extract (OME) and different fractions of OME. Additionally, the antioxidant and antiallergic activities of the OME fractions were evaluated. The results showed that the ethyl acetate-soluble fraction of OME has potential antioxidant activity, whereas the n-hexane-soluble fraction showed the strongest inhibition of β-hexosaminidase, which is one of the key factors in allergic reactions. It was concluded that phenolic compounds might contribute to the antioxidant activity while unsaturated fatty acids contribute to the antiallergy activity.


2017 ◽  
Vol 31 (2) ◽  
pp. 1650-1664 ◽  
Author(s):  
Filip Stankovikj ◽  
Armando G. McDonald ◽  
Gregory L. Helms ◽  
Mariefel V. Olarte ◽  
Manuel Garcia-Perez

Holzforschung ◽  
2008 ◽  
Vol 62 (5) ◽  
Author(s):  
Jorge Rencoret ◽  
Gisela Marques ◽  
Ana Gutiérrez ◽  
David Ibarra ◽  
Jiebing Li ◽  
...  

Abstract The chemical structure of milled-wood lignins from Eucalyptus globulus, E. nitens, E. maidenii, E. grandis, and E. dunnii was investigated. The lignins were characterized by analytical pyrolysis, thioacidolysis, and 2D-NMR that confirmed the predominance of syringyl over guaiacyl units and only showed traces of p-hydroxyphenyl units. E. globulus lignin had the highest syringyl content. The heteronuclear single quantum correlation (HSQC) NMR spectra yielded information about relative abundances of inter-unit linkages in the whole polymer. All the lignins showed a predominance of β-O-4′ ether linkages (66–72% of total side-chains), followed by β-β′ resinol-type linkages (16–19%) and lower amounts of β-5′ phenylcoumaran-type (3–7%) and β-1′ spirodienone-type linkages (1–4%). The analysis of desulfurated thioacidolysis dimers provided additional information on the relative abundances of the various carbon-carbon and diaryl ether bonds, and the type of units (syringyl or guaiacyl) involved in each of the above linkage types. Interestingly, 93–94% of the total β-β′ dimers included two syringyl units indicating that most of the β-β′ substructures identified in the HSQC spectra were of the syringaresinol type. Moreover, three isomers of a major trimeric compound were found which were tentatively identified as arising from a β-β′ syringaresinol substructure attached to a guaiacyl unit through a 4-O-5′ linkage.


2017 ◽  
Vol 9 (1) ◽  
pp. 79
Author(s):  
Sri Wahdaningsih ◽  
Subagus Wahyuono ◽  
Sugeng Riyanto ◽  
Retno Murwanti

<p> </p><p>Red dragon fruit (<em>H. Polyrhizus</em>) is one of the the plants that has a great potential as natural antioxidant. This study tested the activity of radical scavenging of 2-2' diphenyl -1- pikril hidrazil (DPPH) in the methanol extract, as well as in the soluble and insoluble fractions of ethyl acetate of red dragon fruit peel. This research is carried out through various stages, such as: extraction and fractionation to obtain both insoluble fraction and soluble fractions of ethyl acetate. Antioxidant activity test is conducted by the method of thin layer chromatography and spectrophotometry.<strong> </strong>Antioxidant activity test, IC<sub>50 </sub>values of methanol extract, ethyl acetate soluble fraction, and insoluble fraction of ethyl acetate had been obtained consecutively as much as 241.19 µg /mL, 8.34  µg/mL, 46.84 µg/mL. The soluble fraction of ethyl acetate had greater antioxidant activity compared to the methanol extract and the insoluble fractions of ethyl acetate.</p>


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