Differences in physicochemical properties of pectin extracted from pomelo peel with different extraction techniques.

In order to obtain high yield pomelo peel pectin with better physicochemical properties, four pectin extraction methods, including hot acid extraction (HAE), microwave-assisted extraction (MAE), ultrasound-assisted extraction, and enzymatic assisted extraction (EAE) were compared. MAE led to the highest pectin yield (20.43%), and the lowest pectin recovery was found for EAE (11.94%). The physicochemical properties of pomelo peel pectin obtained by different methods were also significantly different. Pectin samples obtained by MAE had the highest methoxyl content (8.35%), galacturonic acid content (71.36%), and showed a higher apparent viscosity, thermal and emulsion stability. The pectin extracted by EAE showed the highest total phenolic content (12.86%) and lowest particle size (843.69 nm), showing higher DPPH and ABTS scavenging activities than other extract methods. The pectin extracted by HAE had the highest particle size (966.12 nm) and degree of esterification (55.67%). However, Fourier-transform infrared spectroscopy showed that no significant difference occurred among the different methods in the chemical structure of the extracted pectin. This study provides a theoretical basis for the industrial production of pomelo peel pectin.

Ultrasonic-assisted extraction to enhance the recovery of bioactive phenolic compounds from Commiphora gileadensis leaves.

The "ultrasonic-assisted extraction (UAE)" method was utilized in this work to assess how different process parameters affected the yield and recovery of phenolic compounds from the leaf of Commiphora gileadensis, which is one of the medicinal plants with a variety of biological functions. Its leaf is used for a various of therapeutic applications, such as the treatment of bacterial infections, inflammation, and wound healing. The "One-Factor-At-a-Time (OFAT)" approach was employed to examine the impacts of various UAE process parameters on the process of extraction, which include time of extraction, sample/solvent ratio, ultrasonic frequency, and solvent (ethanol) concentration. The extracts were then investigated for the presence of several phytochemicals using analytical techniques such as "Gas Chromatography-Mass Spectroscopy (GC-MS)" and "Fourier Transform Infrared Spectroscopy (FTIR)" studies. The findings showed that the maximum extraction yield, the total phenolic content (TPC), and the total flavonoids content (TFC) of the ethanolic extract of the leaves of C. gileadensis using the UAE method were at 31.80 ± 0.41 %, 96.55 ± 2.81 mg GAE/g d.w. and 31.66 ± 2.01 mg QE/g d.w. accordingly under a procedure duration of 15 min, ultrasonic frequency of 20 kHz, solvent/sample ratio of 1:20 g/mL, and solvent concentration of 40 % v/v. The leaves extract of C. gileadensis included 25 phenolic compounds that were previously unreported, and GC-MS analysis confirmed their presence. Hence, it follows that the UAE technique can successfully extract the phytochemicals from C. gileadensis for a variety of therapeutic uses.

Sustainable green extraction of anthocyanins and carotenoids using deep eutectic solvents (DES): A review of recent developments.

Recently, deep eutectic solvents (DES) have been extensively researched as a more biocompatible and efficient alternative to conventional solvents for extracting pigments from natural resources. The efficiency of DES extraction for the anthocyanin and carotenoid can be enhanced by microwave-assisted extraction (MAE) and/or ultrasound-assisted extraction (UAE) techniques. Apart from the extraction efficiency, the toxicity and recovery of the pigments and their bioavailability are crucial for potential applications. A plethora of studies have explored the extraction efficiency, toxicity, and recovery of pigments from various natural plant-based matrices using DES. Nevertheless, a detailed review of the deep eutectic solvent extraction of natural pigments has not been reported to date. Additionally, the toxicity, safety, and bioavailability of the extracted pigments, and their potential applications are not thoroughly documented. Therefore, this review is designed to understand the aforementioned concepts in using DES for anthocyanin and carotenoid extraction.

Fibrillization of lentil proteins is impacted by the protein extraction conditions and co-extracted phenolics.

Legume proteins can be induced to form amyloid-like fibrils upon heating at low pH, with the exact conditions greatly impacting the fibril characteristics. The protein extraction method may also impact the resulting fibrils, although this effect has not been carefully examined. Here, the fibrillization of lentil protein prepared using various extraction methods and the corresponding fibril morphology were characterized. It was found that an acidic, rather than alkaline, protein extraction method was better suited for producing homogeneous, long, and straight fibrils from lentil proteins. During alkaline extraction, co-extracted phenolic compounds bound proteins through covalent and non-covalent interactions, contributing to the formation of heterogeneous, curly, and tangled fibrils. Recombination of isolated phenolics and proteins (from acidic extracts) at alkaline pH resulted in a distinct morphology, implicating a role for polyphenol oxidase also in modifying proteins during alkaline extraction. These results help disentangle the complex factors affecting legume protein fibrillization.

Ultrasonic-assisted extraction of grape seed procyanidins, preparation of liposomes, and evaluation of their antioxidant capacity.

The residue remaining after oil extraction from grape seed contain abundant procyanidins. An ultrasonic-assisted enzyme method was performed to achieve a high extraction efficiency of procyanidins when the optimal extraction conditions were 8 U/g of cellulase, ultrasound power of 200 W, ultrasonic temperature of 50 ℃, and ultrasonic reaction time of 40 min. The effects of free procyanidins on both radical scavenging activity and thermal stability at 40, 60, and 80 ℃ of the procyanidins-loaded liposomal systems prepared by the ultrasonic-assisted method were discussed. The presence of procyanidins at concentrations ranging from 0.02 to 0.10 mg/mL was observed to be effective at inhibiting lipid oxidation by 15.15 % to 69.70 % in a linoleic acid model system during reaction for 168 h, as measured using the ferric thiocyanate method. The procyanidins-loaded liposomal systems prepared by the ultrasonic-assisted method were characterized by measuring the mean particle size and encapsulation efficiency. Moreover, the holographic plots showed that the effect-response points of procyanidins combined with α-tocopherol in liposomes were lower than the addition line and 95 % confidence interval limits. At the same time, there were significant differences between the theoretical IC50add value and the experimental IC50mix value. The interaction index (γ) of all combinations was observed to be less than 1. These results indicated that there was a synergistic antioxidant effect between procyanidins combined with α-tocopherol, which will show promising prospects in practical applications. In addition, particle size differentiation and morphology agglomeration were observed at different time points of antioxidant activity determination (0, 48, 96 h).

Toward well-defined colloidal particles: Efficient fractionation of lignin by a multi-solvent strategy.

Colloidal lignin particles (CLPs) have sparked various intriguing insights toward bio-polymeric materials and triggered many lignin-featured innovative applications. Here, we report a multi-solvent sequential fractionation methodology integrating green solvents of acetone, 1-butanol, and ethanol to fractionate industrial lignin for CLPs fabrication. Through a rationally designed fractionation strategy, multigrade lignin fractions with variable hydroxyl group contents, molecular weights, and high purity were obtained without altering their original chemical structures. CLPs with well-defined morphology, narrow size distribution, excellent thermal stability, and long-term colloidal stability can be obtained by rational selection of lignin fractions. We further elucidated that trace elements (S, N) were reorganized onto the near-surface area of CLPs from lignin fractions during the formation process in the form of -SO42- and -NH2. This work provides a sustainable and efficient strategy for refining industrial lignin into high-quality fractions and an in-depth insight into the CLPs formation process, holding great promise for enriching the existing libraries of colloidal materials.

Ultrasound assisted wall-breaking extraction and primary structures, bioactivities, rheological properties of novel Exidia yadongensis polysaccharide.

New natural multifunctional polysaccharide and its innovatory extraction technology may be urgently needed for food industries. Our aims were to establish new extraction method and investigate the primary structures, bioactivities and rheological properties of novel E. yadongensis polysaccharide (EYP). Ultrasound assisted mechanical wall-breaking extraction (MAUE) was successfully established for the EYP extraction from a new E. yadongensis. Based on the MAUE with RSM, the polysaccharide yield of 17.92 ± 0.56 % with the optimal parameters of five extraction factors were obtained, and current MAUE was characterized by its high yield, low extraction temperature and short ultrasound time. After the isolation and purification, the EYP as a protein-bound polysaccharide was obtained. FT-IR and NMR analysis showed that the main backbone of the EYP comprised of (1 â†’ 4)-ß-D-glucopyranosyl and (1 â†’ 6)-ɑ-D-mannopyranosyl groups; EYP exhibited significant antioxidant, antibacterial, antitumor, antidiabetic activities, and good viscoelastic properties in low pH solutions (P < 0.05). The EYP may be used as a natural functional and cohesive agent in food industries.

Dry fractionation process operations in the production of protein concentrates: A review.

The market for plant proteins is expanding rapidly as the negative impacts of animal agriculture on the environment and resources become more evident. Plant proteins offer competitive advantages in production costs, energy requirements, and sustainability. Conventional plant-protein extraction is water and chemical-intensive, posing environmental concerns. Dry fractionation is an energy-efficient and environmentally friendly process for protein separation, preserving protein's native functionality. Cereals and pulses are excellent sources of plant proteins as they are widely grown worldwide. This paper provides a comprehensive review of the dry fractionation process utilized for different seeds to obtain protein-rich fractions with high purity and functionality. Pretreatments, such as dehulling and defatting, are known to enhance the protein separation efficiency. Factors, such as milling speed, mill classifier speed, feed rate, seed type, and hardness, were crucial for obtaining parent flour of desired particle size distribution during milling. The air classification or electrostatic separation settings are crucial in determining the quality of the separated protein. The cut point in air classification is targeted based on the starch granule size of the seed material. Optimization of these operations, applied to different pulses and seeds, led to higher yields of proteins with higher purity. Dual techniques, such as air classification and electrostatic separation, enhance protein purity. The yield of the protein concentrates can be increased by recycling the coarse fractions. Further research is necessary to improve the quality, purity, and yield of protein concentrates to enable more efficient use of plant proteins to meet global protein demands.

Reverse flow enhanced inertia pinched flow fractionation.

Particle separation plays a critical role in many biochemical analyses. In this article, we report a method of reverse flow enhanced inertia pinched flow fractionation (RF-iPFF) for particle separation. RF-iPFF separates particles by size based on the flow-induced inertial lift, and in the abruptly broadened segment, reverse flow is utilized to further enhance the separation distance between particles of different sizes. The separation performance can be significantly improved by reverse flow. Generally, compared with the case without reverse flow, this RF-iPFF technique can increase the particle throughput by about 10 times. To demonstrate the advantages of RF-iPFF, RF-iPFF was compared with traditional iPFF through a control experiment. RF-iPFF consistently outperformed iPFF across various conditions we studied. In addition, we use tumor cells spiked into the human whole blood to evaluate the separation performance of RF-iPFF.

A gas phase fractionation acquisition scheme integrating ion mobility for rapid diaPASEF library generation.

Data independent acquisition (DIA/SWATH) MS is a primary strategy in quantitative proteomics. diaPASEF is a recent adaptation using trapped ion mobility spectrometry (TIMS) to improve selectivity/sensitivity. Complex DIA spectra are typically analyzed with reference to spectral libraries. The best-established method for generating libraries uses offline fractionation to increase depth of coverage. More recently strategies for spectral library generation based on gas phase fractionation (GPF), where a representative sample is injected serially using narrow DIA windows that cover different mass ranges of the complete precursor space, have been introduced that performed comparably to deep offline fractionation-based libraries. We investigated whether an analogous GPF-based approach that accounts for the ion mobility (IM) dimension is useful for the analysis of diaPASEF data. We developed a rapid library generation approach using an IM-GPF acquisition scheme in the m/z versus 1/K0 space requiring seven injections of a representative sample and compared this with libraries generated by direct deconvolution-based analysis of diaPASEF data or by deep offline fractionation. We found that library generation by IM-GPF outperformed direct library generation from diaPASEF and had performance approaching that of the deep library. This establishes the IM-GPF scheme as a pragmatic approach to rapid library generation for analysis of diaPASEF data.

Capillary Electrophoresis Plasma Fractionation for Lipids Analysis.

Extraction of lipids has mainly used density liquid phase separation techniques; however, these methods are limited by their broad extraction and lack specificity. Complex mixtures like blood plasma contain multiple lipid classes, whose distribution in the body are mediated by protein-lipid interactions and integration of lipids in larger lipoprotein complexes. The capillary electrophoresis system separates complex mixtures by electrokinetic forces that preserve protein-lipid complexation and allow for the fractionation of samples. Here we present a methodology for fractionating plasma using the capillary electrophoresis system.

Response surface methodology as a tool to optimize the extraction of bioactive compounds from plant sources.

Response surface methodology (RSM) is a widely used mathematical and statistical technique for modeling and optimizing the process for the extraction of bioactive compounds. This review explains the optimization approach through the use of experimental design and empirical models for response prediction and the utilization of the desirability function for multiple response optimization. This paper also reviews recent studies on the application of RSM to optimize bioactive compound extraction processes such as conventional solvent extraction, microwave-assisted extraction, supercritical fluid extraction, and ultrasound-assisted extraction. Finally, the challenges associated with the use of RSM and the efforts made to improve RSM in the extraction process are also highlighted. Overall, this review informs many aspects of RSM that are occasionally ignored or insufficiently discussed with regard to the optimization of bioactive compound extraction processes, and it summarizes significant applications where RSM proved suitable. © 2022 Society of Chemical Industry.

Updating the status quo on the extraction of bioactive compounds in agro-products using a two-pot multivariate design. A comprehensive review.

Extraction is regarded as the most crucial stage in analyzing bioactive compounds. Nonetheless, due to the intricacy of the matrix, numerous aspects must be optimized during the extraction of bioactive components. Although one variable at a time (OVAT) is mainly used, this is time-consuming and laborious. As a result, using an experimental design in the optimization process is beneficial with few experiments and low costs. This article critically reviewed two-pot multivariate techniques employed in extracting bioactive compounds in food in the last decade. First, a comparison of the parametric screening methods (factorial design, Taguchi, and Plackett-Burman design) was delved into, and its advantages and limitations in helping to select the critical extraction parameters were discussed. This was followed by a discussion of the response surface methodologies (central composite (CCD), Doehlert (DD), orthogonal array (OAD), mixture, D-optimal, and Box-Behnken designs (BBD), etc.), which are used to optimize the most critical variables in the extraction of bioactive compounds in food, providing a sequential comprehension of the linear and complex interactions and multiple responses and robustness tests. Next, the benefits, drawbacks, and possibilities of various response surface methodologies (RSM) and some of their usages were discussed, with food chemistry, analysis, and processing from the literature. Finally, extraction of food bioactive compounds using RSM was compared to artificial neural network modeling with their drawbacks discussed. We recommended that future experiments could compare these designs (BBD vs. CCD vs. DD, etc.) in the extraction of food-bioactive compounds. Besides, more research should be done comparing response surface methodologies and artificial neural networks regarding their practicality and limitations in extracting food-bioactive compounds.

Microporous Matrimid/PIM-1 Thin Film Composite Membranes with Narrow Pore Size Distribution used for Molecular Separation in Organic Solvents.

Polymers of intrinsic microporosity (PIMs) are a class of microporous organic materials that contain interconnected pores of less than 2 nm in diameter. Such materials are of great potential used in membranes for molecular separation, such as drug fractionation in pharmaceutical industry. However, the PIMs membranes are often susceptible to low separation selectivity toward different molecules due to their wide pore size distribution. Herein, a linear polyimide, Matrimid, is incorporated with PIM-1 (a typical member of PIMs) by solution blending, and the blends are dip-coated onto a polyimide P84 support membrane to prepare thin-film composite (TFC) membranes to control pore size distribution while keep high microporosity. The component miscibility, pore characteristics, and molecular separation performances of the Matrimid/PIM-1 TFC membranes are investigated in detail. The Matrimid and PIM-1 are partially miscible due to their similar Hansen solubility parameters. The Matrimid endows the selective layers (coatings) with narrower pore size distribution due to more compact chain packing. The prepared Matrimid/PIM-1 TFC membranes show high selectivity for separation of riboflavin (80% of retention) and isatin (only 5% of retention). The developed membranes exhibit great potential for separating molecules with different molecular weights.

Ultrasonic treatment of foam for the prevention of foam-induced pepsin inactivation.

The phenomenon of foam-induced inactivation is a common challenge during foam fractionation of proteins. In this work, we attempted to use ultrasound to treat foam out of the foam fractionation column with the aim of minimizing the foam-induced protein inactivation using pepsin as a model protein. Firstly, the mechanisms by which ultrasound prevented the foam-induced pepsin inactivation during defoaming were explored. The results showed that ultrasound promoted the refolding of unfolded pepsin molecules at the gas-liquid interface to restore their activities during the desorption process from the interface and before dissolving into the foamate. Subsequently, the effects of ultrasonic power on the pepsin renaturation were analyzed, which revealed that the unfolding degree of pepsin in the foamate gradually decreased and then increased as the ultrasonic power increased. Correspondingly, the specific activity of pepsin in the foamate increased and then decreased. Finally, we explored the effects of defoaming efficiency, type of gas and pH. The results indicated that the decrease in defoaming efficiency and gas solubility in water facilitated the ultrasound-assisted pepsin renaturation in the pH range from 1.0 to 2.5. When air was applied in the foaming process, the specific activity of pepsin in the foamate with ultrasonic treatment was not significantly different from that in the feed solution at ultrasonic power of 400 W and pH 2.0. Collectively, these results indicate the ultrasonic treatment of foam effectively prevented the foam-induced pepsin inactivation.

Effects of different extraction methods on the structural, antioxidant and hypoglycemic properties of red pitaya stem polysaccharide.

Processing conditions can change the compositions and microstructures of polysaccharides, resulting in favorable and unfavorable effects on their chemical characteristics and bioactivites. Here, this study comparatively evaluated the effects of the commonly used hot water, alkaline, acidic, enzymatic, ultrasonic and hot water-alkaline extractions on the structural features and antioxidant and hypoglycemic properties of pitaya stem polysaccharides. Nuclear magnetic resonance spectroscopy showed six polysaccharides had similar glycosyl types. Scanning electron microscopy exhibited the surface morphology of the extracted six polysaccharides differed significantly. Polysaccharide obtained by hot water showed better antioxidant and hypoglycemic properties than that of the other polysaccharides. These data suggested that alkaline, acidic, enzymatic, ultrasonic and hot water-alkaline extractions have various influences on the degradation of polysaccharides without varying the major structure in comparison with hot water extraction. Additionally, monosaccharide composition and molecular weight of polysaccharides are two chief factors affecting the bioactivity of pitaya stem polysaccharides.

An integral method for determining the molecular composition of lignin and its application.

Lignin is a natural and renewable aromatic polymer, but only about 2% of lignin is utilized with high added value. Polydispersity and heterogeneity are the key reasons for the difficulty in separation, fractionation, characterization, purification and utilization of lignin. However, the molecular weight of lignin is still described from the overall perspective of number-/weight-average molecular weight (Mn and Mw), which if far from enough to understand the heterogeneous and dispersed lignin. To provide a tool for understanding the molecular weight of lignin from a molecular perspective, an integral method for quantifying the molecular characteristics of lignin molecules at arbitrary molecular intervals on the molecular weight distribution curve of lignin was established. The molecular contents of wheat straw lignin as well as its soluble and insoluble fractions at different intervals were calculated. The ease of fractionation of small molecules with weights lower than 8000 g/mol into soluble fractions, and that of large molecules with weights higher than 10,000 g/mol into insoluble fractions were quantitatively analyzed. The established integral method will significantly help in the understanding the properties of lignin at the molecular-level, as well as the fractionation and utilization of lignin.

Successive organic solvent fractionation and homogenization of technical lignin for polyurethane foam with high mechanical performance.

This work demonstrates an organic solvent fractionation method for lignin homogenization, which can effectively reduce the lignin heterogeneity and use each lignin fraction to prepare polyurethane foams (PUFs) with excellent mechanical properties. Such fractions were fully characterized by GPC, NMR (31P, 2D-HSQC), FTIR, and TG to obtain a detailed description of the structures and properties. The properties of PUFs from each lignin fraction showed higher compatibility than that from unfractionated industrial lignin, as studied by morphology and DSC analysis. The improvement of compatibility between the fractionated lignin fractions and polyethylene glycol can effectively enhance the mechanical properties of the prepared PUFs. The hysteresis loss (43.10%-51.85%) and resilience (95.81%-98.81%) of the fractionated lignin polyurethane foams (LPUFs) were better than that from the unfractionated LPUFs (hysteresis loss 41.64%, resilience 94.67%) at the lignin content of 5%. Subsequently, the strong relationships between lignin structures and PUF properties were demonstrated in detail. The suggested approach provides greater possibilities to prepare LPUFs with tunable properties based on real industrial lignin fractions, rather than modified lignin.

Phase-specific stable isotope fractionation effects during combined gas-liquid phase exchange and biodegradation.

Stable isotope fractionation of toluene under dynamic phase exchange was studied aiming at ascertaining the effects of gas-liquid partitioning and biodegradation of toluene stable isotope composition in liquid-air phase exchange reactors (Laper). The liquid phase consisted of a mixture of aqueous minimal media, a known amount of a mixture of deuterated (toluene-d) and non-deuterated toluene (toluene-h), and bacteria of toluene degrading strain Pseudomonas putida KT2442. During biodegradation experiments, the liquid and air-phase concentrations of both toluene isotopologues were monitored to determine the observable stable isotope fractionation in each phase. The results show a strong fractionation in both phases with apparent enrichment factors beyond -800‰. An offset was observed between enrichment factors in the liquid and the gas phase with gas-phase values showing a stronger fractionation in the gas than in the liquid phase. Numerical simulation and parameter fitting routine was used to challenge hypotheses to explain the unexpected experimental data. The numerical results showed that either a very strong, yet unlikely, fractionation of the phase exchange process or a - so far unreported - direct consumption of gas phase compounds by aqueous phase microorganisms could explain the observed fractionation effects. The observed effect can be of relevance for the analysis of volatile contaminant biodegradation using stable isotope analysis in unsaturated subsurface compartments or other environmental compartment containing a gas and a liquid phase.

Transformation and stable isotope fractionation of the urban biocide terbutryn during biodegradation, photodegradation and abiotic hydrolysis.

Terbutryn is a widely used biocide in construction materials like paint and render to prevent the growth of microorganisms, algae and fungi. Terbutryn is released from the facades into the environment during rainfall, contaminating surface waters, soil and groundwater. Knowledge of terbutryn dissipation from the facades to aquatic ecosystems is scarce. Here, we examined in laboratory microcosms degradation half-lives, formation of transformation products and carbon and nitrogen isotope fractionation during terbutryn direct (UV light with λ = 254 nm and simulated sunlight) and indirect (simulated sunlight with nitrate) photodegradation, abiotic hydrolysis (pH = 1, 7 and 13), and aerobic biodegradation (stormwater pond sediment, soil and activated sludge). Biodegradation half-lives of terbutryn were high (>80 d). Photodegradation under simulated sunlight and hydrolysis at extreme pH values indicated slow degradability and accumulation in the environment. Photodegradation resulted in a variety of transformation products, whereas abiotic hydrolysis lead solely to terbutryn-2-hydroxy in acidic and basic conditions. Biodegradation indicates degradation to terbutryn-2-hydroxy through terbutryn-sulfoxide. Compound-specific isotope analysis (CSIA) of terbutryn holds potential to differentiate degradation pathways. Carbon isotope fractionation values (εC) ranged from -3.4 ± 0.3‰ (hydrolysis pH 1) to +0.8 ± 0.1‰ (photodegradation under UV light), while nitrogen isotope fractionation values ranged from -1.0 ± 0.4‰ (simulated sunlight photodegradation with nitrate) to +3.4 ± 0.2‰ (hydrolysis at pH 1). In contrast, isotope fractionation during biodegradation was insignificant. ΛN/C values ranged from -1.0 ± 0.1 (hydrolysis at pH 1) to 2.8 ± 0.3 (photodegradation under UV light), allowing to differentiate degradation pathways. Combining the formation of transformation products and stable isotope fractionation enabled identifying distinct degradation pathways. Altogether, this study highlights the potential of CSIA to follow terbutryn degradation in situ and differentiate prevailing degradation pathways, which may help to monitor urban biocide remediation and mitigation strategies.