acidic methanolysis
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Cellulose ◽  
2021 ◽  
Author(s):  
Manuel Becker ◽  
Kyujin Ahn ◽  
Markus Bacher ◽  
Chunlin Xu ◽  
Anna Sundberg ◽  
...  

AbstractKnowledge about the carbohydrate composition of pulp and paper samples is essential for their characterization, further processing, and understanding the properties. In this study, we compare sulfuric acid hydrolysis and acidic methanolysis, followed by GC–MS analysis of the corresponding products, by means of 42 cellulose and polysaccharide samples. Results are discussed and compared to solid-state NMR (crystallinity) and gel permeation chromatography (weight-averaged molecular mass) data. The use of the hydrolysis methods in the context of cellulose conservation science is evaluated, using e-beam treated and artificially aged cellulose samples.



2021 ◽  
Vol 14 (1) ◽  
Author(s):  
Liza A. Wilson ◽  
Fabien Deligey ◽  
Tuo Wang ◽  
Daniel J. Cosgrove

Abstract Background Epidermal cell walls have special structural and biological roles in the life of the plant. Typically they are multi-ply structures encrusted with waxes and cutin which protect the plant from dehydration and pathogen attack. These characteristics may also reduce chemical and enzymatic deconstruction of the wall for sugar analysis and conversion to biofuels. We have assessed the saccharide composition of the outer epidermal wall of onion scales with different analytical methods. This wall is a particularly useful model for cell wall imaging and mechanics. Results Epidermal walls were depolymerized by acidic methanolysis combined with 2M trifluoracetic acid hydrolysis and the resultant sugars were analyzed by high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD). Total sugar yields based on wall dry weight were low (53%). Removal of waxes with chloroform increased the sugar yields to 73% and enzymatic digestion did not improve these yields. Analysis by gas chromatography/mass spectrometry (GC/MS) of per-O-trimethylsilyl (TMS) derivatives of the sugar methyl glycosides produced by acidic methanolysis gave a high yield for galacturonic acid (GalA) but glucose (Glc) was severely reduced. In a complementary fashion, GC/MS analysis of methyl alditols produced by permethylation gave substantial yields for glucose and other neutral sugars, but GalA was severely reduced. Analysis of the walls by 13C solid-state NMR confirmed and extended these results and revealed 15% lipid content after chloroform extraction (potentially cutin and unextractable waxes). Conclusions Although exact values vary with the analytical method, our best estimate is that polysaccharide in the outer epidermal wall of onion scales is comprised of homogalacturonan (~ 50%), cellulose (~ 20%), galactan (~ 10%), xyloglucan (~ 10%) and smaller amounts of other polysaccharides. Low yields of specific monosaccharides by some methods may be exaggerated in epidermal walls impregnated with waxes and cutin and call for cautious interpretation of the results.



2021 ◽  
Author(s):  
Liza A. Wilson ◽  
Fabien Deligey ◽  
Tuo Wang ◽  
Daniel J. Cosgrove

AbstractBackgroundEpidermal cell walls have special structural and biological roles in the life of the plant. Typically they are multi-ply structures encrusted with waxes and cutin which protect the plant from dehydration and pathogen attack. These characteristics may also reduce chemical and enzymatic deconstruction of the wall for sugar analysis and conversion to biofuels. We have assessed the saccharide composition of the outer epidermal wall of onion scales with different analytical methods. This wall is a particularly useful model for cell wall imaging and mechanics.ResultsEpidermal walls were depolymerized by acidic methanolysis combined with 2 M trifluoracetic acid hydrolysis and the resultant sugars were analyzed by high-performance anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD). Total sugar yields based on wall dry weight were low (53%). Removal of waxes with chloroform increased the sugar yields to 73% and enzymatic digestion did not improve these yields. Analysis by gas chromatography/mass spectrometry (GC/MS) of per-O-trimethylsilyl (TMS) derivatives of the sugar methyl glycosides produced by acidic methanolysis gave a high yield for galacturonic acid (GalA) but glucose (Glc) was severely reduced. In a complementary fashion, GC/MS analysis of methyl alditols produced by permethylation gave substantial yields for glucose and other neutral sugars, but GalA was severely reduced. Analysis of the walls by 13C solid-state NMR confirmed and extended these results and revealed 15% lipid content after chloroform extraction (potentially cutin and unextractable waxes).ConclusionsAlthough exact values vary with the analytical method, our best estimate is that polysaccharide in the outer epidermal wall of onion scales is comprised of homogalacturonan (~50%), cellulose (~20%), galactan (~10%), xyloglucan (~10%) and smaller amounts of other polysaccharides. Low yields of specific monosaccharides by some methods may be exaggerated in epidermal walls impregnated with waxes and cutin and call for cautious interpretation of the results.



2020 ◽  
Vol 1619 ◽  
pp. 460955 ◽  
Author(s):  
Pierluigi Delmonte ◽  
Xabier Belaunzaran ◽  
Clark D. Ridge ◽  
Noelia Aldai ◽  
John K.G. Kramer


2014 ◽  
Vol 83 (3) ◽  
pp. 239-241 ◽  
Author(s):  
Rosália Rubel ◽  
Leandro Freire Dos Santos ◽  
Herta Stutz Dalla Santa ◽  
Luciana Porto de Souza Vandenberghe ◽  
Adenise Lorenci Woiciechowski ◽  
...  

The evaluation of glycosyl composition is an essential step to guide future research designs applied in bioactivity. In the same way, the unexplored potential bioactivity of exopolysaccharide from <em>Ganoderma lucidum</em> is huge. Therefore, this study investigated the glycosyl composition of the exopolysaccharide isolated from submerged fermentation of <em>G. lucidum</em> to serve as guide for future studies on bioactivity. Glycosyl content and composition were evaluated by combined GC/MS of the TMS derivatives of the monosaccharide methyl glycosides produced from the sample by acidic methanolysis. Glycosyl composition analysis showed that the dominant carbohydrate component in all samples of exopolysaccharide isolated from submerged fermentation of <em>G. lucidum</em> CG 144 was glucose (58.1%), mannose (26.6%) and galactose (12.5%) which can be referred to as heteroglycan. These results suggest that this <em>Ganoderma</em> exopolysaccharide may be a new immunomodulatory agent.







2002 ◽  
Vol 57 (11-12) ◽  
pp. 1035-1041 ◽  
Author(s):  
Henning Bubert ◽  
Jörg Lambert ◽  
Stefan Steuernagel ◽  
Friedhelm Ahlers ◽  
Rolf Wiermann

Sporopollenin from the pollen of Typha angustifolia L. was exposed to a series of 36 subsequent acidic methanolysis procedures. The remaining decomposition products were investigated using several spectroscopic methods including Fourier transform infrared spectroscopy (FT-IR), solid state 13C nuclear magnetic resonance spectroscopy (13C-CPMAS-NMR) and X-ray photoelectron spectrometry (XPS). Substantial weight losses of the sporopollenin material occur after each acidic methanolysis step, while FT-IR and 13C-CPMAS-NMR spectra display no noticeable differences after 12, 24 and 36 steps. These findings are interpreted as a hint that the sporopollenin polymer has a uniform composition, i.e. relatively small monomer moieties of similar primary structure are present. Moreover, the weight losses account for the presence of substantial amounts of ether linkages in the sporopollenin polymer.



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