scholarly journals Ambient-Pressured Acid-Catalysed Ethylene Glycol Organosolv Process: Liquefaction Structure–Activity Relationships from Model Cellulose–Lignin Mixtures to Lignocellulosic Wood Biomass

Polymers ◽  
2021 ◽  
Vol 13 (12) ◽  
pp. 1988
Author(s):  
Edita Jasiukaitytė-Grojzdek ◽  
Filipa A. Vicente ◽  
Miha Grilc ◽  
Blaž Likozar

Raising the awareness of carbon dioxide emissions, climate global warming and fossil fuel depletion has renewed the transition towards a circular economy approach, starting by addressing active bio-economic precepts that all portion amounts of wood are valorised as products. This is accomplished by minimizing residues formed (preferably no waste materials), maximizing reaction productivity yields, and optimising catalysed chemical by-products. Within framework structure determination, the present work aims at drawing a parallel between the characterisation of cellulose–lignin mixture (derived system model) liquefaction and real conversion process in the acidified ethylene glycol at moderate process conditions, i.e., 150 °C, ambient atmospheric pressure and potential bio-based solvent, for 4 h. Extended-processing liquid phase is characterized considering catalyst-transformed reactant species being produced, mainly recovered lignin-based polymer, by quantitative 31P, 13C and 1H nuclear magnetic resonance (NMR) spectroscopy, as well as the size exclusion- (SEC) or high performance liquid chromatography (HPLC) separation for higher or lower molecular weight compound compositions, respectively. Such mechanistic pathway analytics help to understand the steps in mild organosolv biopolymer fractionation, which is one of the key industrial barriers preventing a more widespread manufacturing of the biomass-derived (hydroxyl, carbonyl or carboxyl) aromatic monomers or oligomers for polycarbonates, polyesters, polyamides, polyurethanes and (epoxy) resins.

2009 ◽  
Vol 27 (No. 5) ◽  
pp. 386-391 ◽  
Author(s):  
R. Amarowicz ◽  
R.B. Pegg ◽  
A. Kosińska

Phenolic compounds were extracted from bearberry (<i>Arctostaphylos uva-ursi</i> L. Sprengel) leaves into 95% (v/v) ethanol. The tannin constituents were separated from the crude extract using Sephadex LH-20 column chromatography with 95% (v/v) ethanol and 50% (v/v) acetone as the mobile phases. Myosin was isolated and purified from excised pork knuckle muscles using the standard salt-solution extraction procedure followed by gel filtration chromatography. Myosin was precipitated from the solution with bearberry-leaf tannins at pH 5.0. The recovered complex was washed, lyophilised, and subjected to size-exclusion high performance liquid chromatography (SE-HPLC). Based on the basic conditions of the HPLC analysis, a portion of the tannin constituents was liberated from the complex. The UV spectra of these compounds were characterized by a maximum at ~ 300 nm. A portion of the tannins was present in the complex with myosin, and this was confirmed by UV spectra.


2017 ◽  
Vol 11 (3) ◽  
Author(s):  
L. Kaprelyants ◽  
O. Zhurlova ◽  
T. Shpyrko ◽  
L. Pozhitkova

The current study is a review of characteristics, production, physiological properties and application of xylooligosaccharides (XOS). XOS are the carbohydrates, their molecules are built from xylose residues linked mainly by в-(1→4)-glycoside bonds. Xylan is important for plant cell walls and is widely spread component in agricultural by-products. XOS are products of xylan hydrolytic degradation, and exhibiting the high prebiotic potential. The XOS preparation of wheat and rye bran stimulated the cells accumulation ‑ 1,4∙1010 CFU/cm3 of L. аcidophilus and 9,2∙1010 CFU/cm3 of В. bifidum. A difference in XOS molecules branching causes a wide range of their physiological properties: antioxidant, immunomodulation, antimicrobial, anti-inflammatory, anticarcinogenic. XOS can reduce high cholesterol level and triglycerides in blood plasma. XOS application reviewed in this article opens new perspectives on its potential use for human consumption. The rich sources of xylan are wheat, rye and barley bran, rice husk, wheat straw, corncobs, cotton stalk. Industrial way of XOS production includes chemical or enzymatic hydrolysis with following purification. Chemical methods are based on hydrothermal pretreatment and acidic or alkali extraction. Obtained oligosaccharides have a wide range of polymerization degree (DP) from 2 to 20. Enzymatic methods include fermentation with xylanase that allow controlling the XOS accumulation with certain DP. The different chromatographic purification after hydrolysis is used for analytical purposes. There are anion-exchange, size-exclusion, affinity, size-exclusion high-performance liquid chromatography. In addition, biomethods are preferred for XOS used in food, because such preparations do not contain monosaccharides and furfural as contaminants. XOS are stable in a wide range of temperature and pH, justifying the development of new synbiotics generation. Most widely XOS are used in production of functional products and pharmaceutical preparations. But they are also applied in cosmetic, agricultural and mixed feed industries.


2002 ◽  
Vol 2 (5-6) ◽  
pp. 427-433 ◽  
Author(s):  
J. van Leeuwen ◽  
C. Chow ◽  
R. Fabris ◽  
N. Withers ◽  
D. Page ◽  
...  

To gain an improved understanding of the types of organic compounds that are recalcitrant to water treatment, natural organic matter (NOM) isolates from two drinking water sources (Mt. Zero and Moorabool reservoirs, Victoria, Australia) were separated into fractions of distinct chemical behaviour using resins. Four fractions were obtained from each water source and were organics absorbed to: (1) XAD-8 (very hydrophobic acids, VHA); (2) DAX-4 (slightly hydrophobic acids, SHA); (3) bound to an anion exchange resin (charged organics, CHAR); and (4) not absorbed or bound to resins (neutrals, NEUT). These fractions were then tested to determine the capacity of alum to remove them from water and to correlate this with the character of each isolate. The fractions were characterised by the application of high performance size exclusion chromatography (HPSEC), bacterial regrowth potential (BRP), trihalomethane formation potential (THMFP), pyrolysis gas-chromatography mass spectrometry (Py-GC-MS) and thermochemolysis. The highest removals of dissolved organic carbon (DOC) by alum treatment were in waters spiked with the CHAR fractions while the NEUT fractions were the most recalcitrant. The number average molecular weights (Mn) of DOC of the CHAR fractions before treatment were the highest, whilst those of the NEUT fractions were the lowest. After alum treatment, the Mn of the NEUT fractions were only slightly reduced. Results from Py-GC-MS and thermochemolysis indicate that the NEUT fractions had the highest relative proportion of saccharide derived organic material. Nonetheless, the BRP of waters spiked with the NEUT fractions differed markedly, indicating that organics recalcitrant to alum treatment can vary substantially in their chemical composition and capacity to support microbial growth.


Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4545
Author(s):  
Sudharsan Sadhasivam ◽  
Omer Barda ◽  
Varda Zakin ◽  
Ram Reifen ◽  
Edward Sionov

Patulin (PAT) and citrinin (CTN) are the most common mycotoxins produced by Penicillium and Aspergillus species and are often associated with fruits and fruit by-products. Hence, simple and reliable methods for monitoring these toxins in foodstuffs are required for regular quality assessment. In this study, we aimed to establish a cost-effective method for detection and quantification of PAT and CTN in pome fruits, such as apples and pears, using high-performance liquid chromatography (HPLC) coupled with spectroscopic detectors without the need for any clean-up steps. The method showed good performance in the analysis of these mycotoxins in apple and pear fruit samples with recovery ranges of 55–97% for PAT and 84–101% for CTN, respectively. The limits of detection (LOD) of PAT and CTN in fruits were 0.006 µg/g and 0.001 µg/g, while their limits of quantification (LOQ) were 0.018 µg/g and 0.003 µg/g, respectively. The present findings indicate that the newly developed HPLC method provides rapid and accurate detection of PAT and CTN in fruits.


AMB Express ◽  
2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Miriam F. Suzuki ◽  
Larissa A. Almeida ◽  
Stephanie A. Pomin ◽  
Felipe D. Silva ◽  
Renan P. Freire ◽  
...  

AbstractThe human prolactin antagonist Δ1-11-G129R-hPRL is a 21.9 kDa recombinant protein with 188 amino acids that downregulates the proliferation of a variety of cells expressing prolactin receptors. Periplasmic expression of recombinant proteins in E. coli has been considered an option for obtaining a soluble and correctly folded protein, as an alternative to cytoplasmic production. The aim of this work was, therefore, to synthesize for the first time, the Δ1-11-G129R-hPRL antagonist, testing different activation temperatures and purifying it by classical chromatographic techniques. E. coli BL21(DE3) strain was transformed with a plasmid based on the pET25b( +) vector, DsbA signal sequence and the antagonist cDNA sequence. Different doses of IPTG were added, activating under different temperatures, and extracting the periplasmic fluid via osmotic shock. The best conditions were achieved by activating at 35 °C for 5 h using 0.4 mM IPTG, which gave a specific expression of 0.157 ± 0.015 μg/mL/A600 at a final optical density of 3.43 ± 0.13 A600. Purification was carried out by nickel-affinity chromatography followed by size-exclusion chromatography, quantification being performed via high-performance size-exclusion chromatography (HPSEC). The prolactin antagonist was characterized by SDS-PAGE, Western blotting, reversed-phase high-performance liquid chromatography (RP-HPLC) and MALDI-TOF–MS. The final product presented > 95% purity and its antagonistic effects were evaluated in vitro in view of potential clinical applications, including inhibition of the proliferation of cancer cells overexpressing the prolactin receptor and specific antidiabetic properties, taking also advantage of the fact that this antagonist was obtained in a soluble and correctly folded form and without an initial methionine.


Antioxidants ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Urška Jug ◽  
Katerina Naumoska ◽  
Irena Vovk

The antioxidant activities of Japanese knotweed rhizome bark extracts, prepared with eight different solvents or solvent mixtures (water, methanol, 80% methanol(aq), acetone, 70% acetone(aq), ethanol, 70% ethanol(aq), and 90% ethyl acetate(aq)), were determined using a 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical-scavenging assay. Low half maximal inhibitory concentration (IC50) values (2.632–3.720 µg mL−1) for all the extracts were in the range of the IC50 value of the known antioxidant ascorbic acid at t0 (3.115 µg mL−1). Due to the highest extraction yield (~44%), 70% ethanol(aq) was selected for the preparation of the extract for further investigations. The IC50 value calculated for its antioxidant activity remained stable for at least 14 days, while the IC50 of ascorbic acid increased over time. The stability study showed that the container material was of great importance for the light-protected storage of the ascorbic acid(aq) solution in a refrigerator. Size exclusion–high-performance liquid chromatography (SEC-HPLC)–UV and reversed phase (RP)-HPLC-UV coupled with multistage mass spectrometry (MSn) were developed for fractionation of the 70% ethanol(aq) extract and for further compound identification, respectively. In the most potent antioxidant SEC fraction, determined using an on-line post-column SEC-HPLC-DPPH assay, epicatechin, resveratrol malonyl hexoside, and its in-source fragments (resveratrol and resveratrol acetyl hexoside) were tentatively identified by RP-HPLC-MSn. Moreover, epicatechin was additionally confirmed by two orthogonal methods, SEC-HPLC-UV and high-performance thin-layer chromatography (HPTLC) coupled with densitometry. Finally, the latter technique enabled the identification of (−)-epicatechin. (−)-Epicatechin demonstrated potent and stable time-dependent antioxidant activity (IC50 value ~1.5 µg mL−1) for at least 14 days.


Biomedicines ◽  
2020 ◽  
Vol 8 (7) ◽  
pp. 209 ◽  
Author(s):  
Lulu Wu ◽  
Athanasios Mantas ◽  
Simon Gustafsson ◽  
Levon Manukyan ◽  
Albert Mihranyan

This study is dedicated to the rapid removal of protein aggregates and viruses from plasma-derived human serum albumin (HSA) product to reduce the risk of viral contamination and increase biosafety. A two-step filtration approach was implemented to first remove HSA aggregates and then achieve high model virus clearance using a nanocellulose-based filter paper of different thicknesses, i.e., 11 μm (prefilter) and 22 μm (virus filter) at pH 7.4 and room temperature. The pore size distribution of these filters was characterized by nitrogen gas sorption analysis. Dynamic light scattering (DLS) and size-exclusion high performance liquid chromatography (SE-HPLC) were performed to analyze the presence of HSA aggregates in process intermediates. The virus filter showed high clearance of a small-size model virus, i.e., log10 reduction value (LRV) > 5, when operated at 3 and 5 bar, but a distinct decrease in LRV was detected at 1 bar, i.e., LRV 2.65–3.75. The throughput of HSA was also dependent on applied transmembrane pressure as was seen by Vmax values of 110 ± 2.5 L m−2 and 63.6 ± 5.8 L m−2 at 3 bar and 5 bar, respectively. Protein loss was low, i.e., recovery > 90%. A distribution of pore sizes between 40 nm and 60 nm, which was present in the prefilter and absent in the virus filter, played a crucial part in removing the HSA aggregates and minimizing the risk of virus filter fouling. The presented results enable the application of virus removal nanofiltration of HSA in bioprocessing as an alternative to virus inactivation methods based, e.g., on heat treatment.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Xuemei Ma ◽  
Jiayi Yu ◽  
Jing Jing ◽  
Qian Zhao ◽  
Liyong Ren ◽  
...  

AbstractPectin is a kind of natural and complex carbohydrates which is extensively used in food, chemical, cosmetic, and pharmaceutical industries. Fresh sunflower (Helianthus annuus L.) heads were utilized as a novel source of pectin extracted by ammonium oxalate. The conditions of the extraction process were optimized implementing the response surface methodology. Under optimal extraction parameters (extraction time 1.34 h, liquid–solid ratio 15:1 mL/g, ammonium oxalate concentration 0.76% (w/v)), the maximum experimental yield was 7.36%. The effect of spray-drying and freeze-drying on the physiochemical properties, structural characteristics, and antioxidant activities was investigated by FT-IR spectroscopy, high performance size exclusion chromatography, and X-ray diffraction. The results showed freeze-drying lead to decrease in galacturonic acid (GalA) content (76.2%), molecular weight (Mw 316 kDa), and crystallinity. The antioxidant activities of pectin were investigated utilizing the in-vitro DPPH and ABTS radical-scavenging systems. This study provided a novel and efficient extraction method of sunflower pectin, and confirmed that different drying processes had an effect on the structure and properties of pectin.


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