mL Of Solvent Research Articles

Effect of extraction conditions on antioxidant activities of Xanthium strumarium L. sprouts extracts

This research aims to obtain the Xanthium strumarium sprouts extract with the most potent antioxidant activities. The single-factor experiments were used to extract. Factors of extraction, including temperatures (40, 50, 60, and 70°C), time (6, 8, 10, 20, and 30 minutes), and % ethanol in solvent (40, 50, 60, and 70 % EtOH), were applied in the ultrasonic assist extraction of 40°C oven-dried Xanthium strumarium sprouts 1 gram in 25 mL of solvent. Extraction yield (% yield) and % inhibition of active radical DPPH and ABTS were determined, and the correlation to varied factors was analyzed using a statistical program (SPSS). The results showed that, at low temperatures, it would give a low % yield but not affect antioxidant activities. The longer extraction time did not provide a different % yield than the shorter one. The extraction yield is a little better when 50% ethanol is used in water as a solvent and does not affect antioxidant activities. As they observe, we can conclude that the antioxidant activities of extracts do not depend on temperature, time, or % EtOH in solvents. The % inhibition of ABTS radicals is higher than that of DPPH radicals in all experiments, and it can be relied on that the active components in this extract are more polar and favorable to solute in water than EtOH.

Application of Microwave for Core Plug Cleaning

Rock extraction is a particularly major step for the preparation of rock samples for core analysis, it can be performed by many traditional techniques like Soxhlet, centrifuge, and flooding system. In this study, a new technique was suggested for core cleaning by microwave. New experiments were conducted as part of this research project, focusing on the cleaning of several types of core plugs under different conditions such as temperature and solvent volume. Additionally, the goal was to extract hydrocarbons from naturally saturated reservoir rocks that had been prepared for standard testing. These findings were then compared with the conventional method of cleaning samples using an organic solvent, specifically toluene. The experiments successfully employed microwave technology for the cleaning process, effectively optimizing key variables including time, temperature, energy, and solvent quantity. The operational duration was set at 3 hours per day, using 20 ml of solvent, following numerous trials and iterations. This method allowed for the extraction of crude oil from 36 plug samples while achieving complete cleanliness of the rocks. Conducting porosity tests before and after the cleaning procedures showed the absence of any damage to the rock samples. Notably, there was an observed alteration in granular size within an acceptable range of 0.02 to 0.6. Further analyses were conducted, including gas chromatography and infrared analysis, both of which indicated that microwaves had no adverse effect on the crude oil extracted. Conclusively, the use of microwaves in the cleaning of rocks appears as a harmless, economically viable, environmentally friendly technique. The feasibility of this method was proved at the laboratory level, showcasing its potential for wider application.

Titanium Compound Coating on SUS Separator for PEFC By Screen Printing

Currently, the metal separators of polymer electrolyte fuel cells (PEFCs) are mainly made of Ti alloys with press working. According to the report by Strategic Analysis Inc1), Ti separator accounts for a large ratio of the PEFC stack cost. To reduce this cost, it is effective to use inexpensive stainless steel and to apply the coating by screen printing, which is relatively easy to form patterns and less expensive than evaporation or sputtering. However, stainless steel has lower corrosion resistance than that of titanium, and its conductivity decreases in aqueous solution due to the formation of passive film. The purposes of this study are to develop a coating with excellent corrosion resistance and conductivity, as well as adhesion and durability, and to apply the coating on stainless steel by screen-printing. Titanium nitride and titanium carbide were employed as tillers among titanium compounds that have high corrosion resistance and sufficiently low electrical resistivity comparable to that of titanium. As a result of the research, a coating thickness of several hundred micro-m became possible, and it was decided that the gas flow path fabrication would also be done by screen printing.In this experiment, we used titanium nitride powder with different particle sizes, Olycox KC-1300 as binder, and 2-(2-butoxyethoxy) ethyl acetate as solvent to prepare printing pastes. 4 g of binder and 10 mL of solvent were weighed and stirred at 80°C for 12 hours using a magnetic stirrer. 4 g of the stirred solution was mixed with 4 g of titanium nitride powder to form a paste. The paste was screen-printed on SUS304 using a plate simulating a gas flow channel, and then dried at 250°C for 6 hours. The resistance of the coatings prepared by the above method was evaluated after pressure treatment. In addition, anodic polarization was measured in a three-electrode system. The contact resistance was targeted to be less than 10 mΩcm2 , the target value for the contact resistance of PEFC separators, as specified by the U.S. DOE.2) References 1) Mass Production Cost Estimation of Direct H2 PEM Fuel Cell Systems for Transportation Applications: 2017 Update, Brian D. James, Jennie M. Huya-Kouadio, Cassidy Houchins, Daniel A. DeSantis, Strategic Analysis Inc., December 2017.2) Fuel Cell Technologies Multi-Year Research, Development, and Demonstration Plan, U.S. DOE, 2017

Upcycling PET Bottles into P-Doped Hard Carbon Anode Materials for Li-Ion Batteries

Introduction The urgent need to address environmental concerns, particularly the escalating plastic waste crisis, has underscored the importance of exploring innovative methods for enhancing plastic bottle recycling [1]. Among these methods, upcycling—transforming plastic waste into products of greater intrinsic value—has gained significant attention [2, 3].This study focuses on applying upcycling methods to plastic bottles, with a specific emphasis on Polyethylene terephthalate (PET) materials sourced from the Coca-Cola corporation as a case study. PET bottles are chosen due to their widespread use in consumer markets and their prevalence in plastic waste streams.The primary objective of this research is to systematically investigate processes for repurposing PET bottles into hard carbon materials. Such materials hold promise for various applications, notably in energy storage systems like lithium-ion batteries (LIBs). By examining PET dissolution in various solvents, this study aims to identify efficient and sustainable pathways for producing high-quality carbon materials.Additionally, this study integrates phosphorus (P) doping into the synthesis process. P-doping has been demonstrated to enhance the electrochemical performance of carbon materials by altering their electronic and structural properties. The authors successfully synthesized P-doped hard carbon and conducted comprehensive characterization using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and Raman spectroscopy. These analyses provide insights into the effects of doping on the structure and morphology of the resulting hard carbon materials, shedding light on mechanisms behind their improved electrochemical performance.This research aims to contribute to the development of environmentally sustainable solutions for plastic waste management. Through the application of upcycling methods to PET bottles and the integration of P-doping strategies, this study seeks to address the environmental challenges posed by plastic waste while exploring avenues for value-added product creation in advanced technological domains.2. Experimental A novel approach is presented for the synthesis of hard carbon material for lithium-ion batteries (LIBs) utilizing recycled PET bottles from Coca-Cola Classic. The bottles underwent thorough washing with water and ethanol, followed by air drying and cutting into small 3-4 mm square pieces prior to dissolution. Solvents for PET dissolution were prepared by mixing dichloromethane (DCM) with trifluoroacetic acid (TFA) in a volume ratio of 3:7. The PET pieces were dissolved in the solvent mixture at a rate of 2 grams per 10 ml of solvent using a stirrer at 100 rpm for 4 hours. P-doping was achieved by adding phosphoric acid (H3PO4) to the plastic solution in various concentrations (1 mol, 2 mol, 3 mol H3PO4 per 10 ml of solution). The resulting solution was applied as a thin layer (50 μm thick) onto a glass surface and dried in air for 24 hours. Subsequently, the resulting film was annealed in an argon atmosphere at 750°C for 2 hours with a heating rate of 5 degrees/min. The resulting carbon materials were characterized and utilized as anodes for lithium-ion half-cells. Electrochemical properties of the batteries were evaluated using cyclic voltammetry (CV) and galvanostatic charge/discharge methods. This study demonstrates a sustainable and efficient method for the synthesis of carbon materials for LIBs from recycled plastic waste, with promising electrochemical performance. Results and Discussion The XRD analysis presented in Figure 1 demonstrate that the obtained carbon sample possessed the high-quality attributes required for battery-grade hard carbon which is substantiated by the distinct peaks observed. Moreover, the initial discharge capacity stands at an 758.53 mAh/g, accompanied by an initial Coloumbic efficiency of 49.75%. After the 10th cycle the Coulombic efficiency reached 97.98%. The corresponding capacitance values after the 10th and 50th cycle are 338,35 and 304,71 mA.Fig. 1 X-ray diffraction pattern of obtained powder References Olazabal, I., Goujon, N., Mantione, D., Alvarez-Tirado, M., Jehanno, C., Mecerreyes, D., & Sardon, H. (2022). From plastic waste to new materials for energy storage. <i>Polymer Chemistry</i>, <i>13</i>(29), 4222–4229. https://doi.org/10.1039/d2py00592aMirjalili, A., Dong, B., Pena, P., Ozkan, C. S., & Ozkan, M. (2020). Upcycling of polyethylene terephthalate plastic waste to microporous carbon structure for energy storage. <i>Energy Storage</i>, <i>2</i>(6). https://doi.org/10.1002/est2.201Nagmani, & Puravankara, S. (2023). Utilization of PET derived hard carbon as a battery-type, higher plateau capacity anode for sodium-ion and potassium-ion batteries. <i>Journal of Electroanalytical Chemistry</i>, <i>946</i>. https://doi.org/10.1016/j.jelechem.2023.117731 Figure 1

Investigating the Effect of the Yellow Chlorophyll on the Characteristics of Liquid Polyethylene Glycol for Liquid Electrolyte Solar Cells

In this study, polyethylene glycol (PEG) and natural dye were employed to make the liquid electrolyte media for solar cells. To prepare varied amounts of dye, the yellow dye of the flowers was extracted using diluted ethanol via ionized water. To produce a constant concentration of all polymer liquids, 10g of PEG dissolves in 1000 ml of solvents including: (di-water, dilute dye, and concentrated dye) individually. The viscosity of solutions was determined using an Ostwald viscometer at various temperatures. Optical parameters such as transmittance, absorbance, and indirect energy gap were investigated utilizing the ultraviolet spectrum. The results reveal that increasing the temperature causes the viscosity decreases and the solar cell efficiency increases. When the dye concentration is increased, the absorbance and absorption coefficient increase, while the transmittance decreases. After adding the concentrated dye, the energy gap of liquid PEG reduces from 1.4 eV to 0.6 eV. PEG with concentrated dye, on the other hand, is the best sample based on the energy gap value. As a result, four concentrations of PEG liquid were prepared: (0.02, 0.025, and 0.03) w/v concentrations, followed by the addition of the concentration dye in the same quantity for each concentration of PEG liquid. Four prepared liquids were tested for viscosity. The results showed that the viscosity of PEG + concentrated dye decreased as the PEG concentration was increased. When the concentration of PEG solution without dye is increased, the viscosity of PEG liquids increases.

The Optimisation of Ultrasound-Assisted Extraction for the Polyphenols Content and Antioxidant Activity on Sanguisorba officinalis L. Aerial Parts Using Response Surface Methodology

The aim of this study was to optimise ultrasound-assisted extraction (UAE) of the herb Sanguisorba officinalis L. in terms of the antioxidant activity (DPPH and FRAP method) and total polyphenol content (TPC). Optimisation was performed using the response surface methodology (RSM) with a third-degree (33) Central Composite Design (CCD) approach. The RSM was applied to obtain the optimal combination of (1) raw material content (2.25–7.5 g raw material/100 mL of solvent), (2) ethanol concentration (20–60% v/v), and (3) extraction time (1–15 min). The optimal conditions for the extraction of polyphenols and antioxidant potential were a raw material content of 7.5 g/100 mL of solvent (solid/solvent ratio 13.3 mL/g), an ethanol concentration of 47% v/v, and an extraction time of 10 min. At these optimal extraction parameters, the maximum extraction of polyphenols and antioxidant activity obtained experimentally was found to be very close to its predicted value and was 12.9 mmol Trolox/L (DPPH method), 19.4 mmol FeSO4/L (FRAP method), and 2.1 g GA/L (TPC). The mathematical model developed was found to fit with the experimental data on the antioxidant potential and polyphenol extraction. The n-octanol/water partition coefficient of the optimised extract was used to determine their lipophilicity. Our studies have shown that the optimised extract is highly hydrophilic (log P &lt; 0). Optimal parameters can be used for the industrial extraction of the S. officinalis herb for the needs of, among others, the pharmaceutical or cosmetic industry.

Enhanced Extraction of Tanshinones from Salvia miltiorrhiza Using Natural-Surfactant-Based Cloud Point Extraction

Salvia miltiorrhiza (SM) contains the tanshinones, a compound with various pharmacological effects, and has been extensively studied as a pharmaceutical material. However, conventional methods for extracting tanshinones face challenges such as environmental hazards and high cost. In this study, we aimed to effectively extract tanshinones from SM using cloud point extraction (CPE) with lecithin, a natural surfactant. By optimizing various extraction conditions including the solid-to-liquid ratio, lecithin concentration, NaCl concentration, pH, and equilibrium temperature, the optimal extraction efficiency was achieved using 20 mL of solvent per 1 g of sample, 3% lecithin (w/v), 2% NaCl (w/v), pH 6, and room temperature (25 ± 2 °C). The CPE method, which minimizes the use of organic solvent and is eco-friendly, demonstrated improvements in extraction efficiency, with a 4.55% increase for dihydrotanshinone I, 8.32% for cryptotanshinone, 15.77% for tanshinone I, and 6.81% for tanshinone IIA compared to the conventional water extraction method. These results suggest that CPE is a promising, environmentally friendly, and efficient approach for extracting hydrophobic components from pharmacologically active materials such as SM, with potential applications across various fields of natural product extraction.

Studying the Characteristics of Tank Oil Sludge

Oil sludge is one of the main pollutants generated by the oil industry. Due to serious pollution and increasing oil production, problems arise every year in the effective treatment of oil sludge. The current study examines the composition and physicochemical characteristics of oil sludge, as well as traditional and new methods for processing oil sludge. With the tightening of environmental protection requirements, oil sludge quality reduction, recycling, and harmless treatment technologies will become necessary in the future. The primary task was to determine the composition of tank oil sludge, separate it from mechanical impurities, and study the influence of ultrasonic treatment and subsequent atmospheric distillation on the extract. The separation of the concentrate and the composition of the tank oil sludge, using an extracted mixture of hexane and benzene, are considered. The use of modern SEM methods, elemental analysis, NMR analysis, IR, ultrasound, and GC–mass spectrometry made it possible to characterize the organic part of reservoir oil sludge and its distillation products. First, 300 g of tank oil sludge was preheated and mixed with 300 mL of solvent (hexane:benzene = 1:1). After mixing with the solvent, the result mixture was filtered. Then, it was placed in an ultrasonic bath and exposed to ultrasound at a frequency of 100 kHz for 30 min. After processing, it was extracted in a Soxhlet apparatus at a temperature of 65 °C to isolate the extract. The resulting extract was analyzed on a gas chromatograph with mass detection. The composition of the extract was as follows (in %): hexane—83.99; total hydrocarbon isomers—7.12; n-hydrocarbons—2.52; benzene—6.37%. At a temperature of 85 °C, the benzene yield was 65.85%. It has been established that the fractions obtained through the distillation of oil sludge at temperatures of 65–85 °C have improved dissolving capacity. It has also been shown that the use of these fractions promotes an increase in the content of hydrocarbon isomers by 12–13% in the extract composition.

Investigation of mechanisms of sulfamethoxazole adsorption on novel adsorbents developed from reed canary grass

In this work, reed canary grass and activated carbons developed from this biomass were used as novel adsorbents to remove sulfamethoxazole (SMX) from water. Raw biomass adsorbent with the lowest surface area demonstrated the lowest SMX adoption capacity of 20.2 ± 1.6 mg/g and the activated carbon adsorbent with the highest surface area showed the highest adsorption capacity of 160.5 ± 4.2 mg/g. π-π, hydrogen bonding, Lewis acid base, and hydrophobic interactions are the possible mechanisms that could be responsible for adsorption of SMX on the adsorbents. Methanol, hydrochloric acid solution, sodium hydroxide solution, and deionized water were used to desorb SMX from the adsorbent. The results of using 20 mL of solvent at 35 °C showed that methanol could desorb loaded SMX with a higher desorption efficiency (80.1 ± 2%) than the aqueous solvents (9.5-46.5%). Decreasing the temperature to 25 °C decreased the desorption efficiency of methanol to 58.5 ± 1%. By decreasing the methanol volume to 5 mL, SMX desorption efficiency could remain comparable (59.1 ± 1.2%). Reusing the adsorbent in 4 adsorption desorption cycles showed that SMX adsorption capacity reduced from 124.9 ± 3.8 mg/g in the first adsorption cycle to 82.1 ± 2.2 mg/g in the second adsorption cycle and was stable in the third and fourth cycles.

Optimization of a novel Renealmia ligulata (Zingiberaceae) essential oil extraction method through microwave-assisted hydrodistillation

Renealmia is a tropical plant genus within the Zingiberaceae family. In tropical South America, Renealmia plants are known for their therapeutic uses against bone and muscle pain, colds, and to counteract snake bite symptoms. Despite the biomedical importance of Renealmia metabolites, the components of their essential oils (EO) have been scarcely studied, and a cause thereof is the lack of local efficient, inexpensive, and environmentally friendly EO extraction methods. This work addressed the optimization of an EO extraction method from the aerial parts and rhizomes of Renealmia ligulata plants based on microwave-assisted hydrodistillation (MAHD) with an ultrasound-assisted extraction (UAE) pretreatment. Three MAHD extraction variables (radiation power, radiation exposure length, and solvent volume) were studied on their own and in combination using a response surface analysis to determine the value combinations leading to optimal EO yields. The results showed that the best average extraction duration time was 42.5 min, combined with a radiation power of 765 W and a solvent volume 225.9 mL for 30 g of aerial part plant material or 799 W and 145 mL of solvent for 20 g of plant rhizomes. A GC-MS analysis of the obtained R. ligulata EOs revealed that their main component was epi-Eudesmol (28% in plant aerial parts and 13% in rhizomes), which is a molecule of interest considering its reported neuro-protective properties.

A dilute-and-inject liquid-gas chromatography-mass spectrometry method for the analysis of sixteen polycyclic aromatic hydrocarbons in extra-virgin olive oil

BackgroundPolycyclic aromatic hydrocarbons (PAHs) represent a diverse group of organic compounds characterized by the fusion of two or more benzene rings arranged in various structural forms. Due to their harmful effects on human health, it is essential to implement monitoring systems and preventive measures to regulate human exposure. Given the affinity of PAHs for lipids, extensive research has been focused on their presence in vegetable oils. This study aimed to develop an on-line liquid-gas chromatography (LC-GC) method (using tandem mass spectrometry) with minimized solvent consumption for the determination of 16 PAHs in extra-virgin olive oil (EVOO). ResultsA side-by-side comparison of the selected-ion-monitoring and the pseudo multiple-reaction-monitoring (p-MRM) acquisition modes was performed, in terms of specificity and detectability. The results obtained using the p-MRM mode were superior, and for this reason it was selected. The method was linear over the concentration range 1–200 μg kg−1 (except in five cases, over 2–200 and 5–200 μg kg−1 ranges). Accuracy (at the 2 μg kg−1 and 20 μg kg−1 concentration levels) was in the 86.9–109.3 % range, with an RSD <10 %. Intra-day and inter-day precision (at 2 μg kg−1 and 20 μg kg−1 concentration levels) were in the 1.2–9.7 % and 3.2–10.8 % ranges, respectively. For all the PAHs, a negative matrix effect was observed. Three out of sixteen PAHs were detected in three EVOOs (among ten samples), albeit at the low ppb level. Limits of quantification were satisfactory in relation to EU legislation on the presence of PAHs in vegetable oils. SignificanceA dilute-and-inject LC-GC-tandem mass spectrometry method is herein proposed fulfilling EU legislation requirements; sample preparation was very simple, inasmuch that it involved only a dilution step, thus avoiding extraction, clean-up, and thus a high consumption of organic solvents. In fact, considering both oil dilution and the LC mobile phase, less than 8 mL of solvents were used.

Optimization of Ultrasound Assisted Extraction (UAE) Conditions on Vitamin C from Roselle Flower

Roselle plant (Hibiscus sabdariffa L.) has many benefits. Vitamin C is an antioxidant in which the human body required. It contains a high amount of vitamin C. However, vitamin C is susceptible to high temperatures. Proper extraction treatment conditions produce optimum vitamin C. This study aims to determine the optimization of vitamin C in rosella flowers. This research uses UAE with Qsonica type – Q500 (500 W, 20 kHz). Extraction treatment conditions control amplitude, time and amount of solvent. The research method used is a laboratory experiment with the RSM (Response Surface Methodology) type CCD (Central Composite Design) approach. The research method was an experimental laboratory using a CCD (Central Composite Design) via RSM (Response Surface Methodology) with an amplitude level from 20% to 50%, a time level from 10 minutes to 20 minutes, and a ratio of the amount of solvent from 140 mL to 260 mL by weight. The results showed that the length of time and the amount of solvent had a significant effect, while the amplitude had no significant effect. The significant quadratic model at p value 0.05 and R2 0.9221 with optimum UAE conditions in the treatment combination of 50 percent amplitude, 20 minutes of time, and 140 ml of solvent resulted in an optimum vitamin C content of 38.76 mg/100g. This research can be used as a reference to determine the value of vitamin C with different amplitude, time, and amount of solvent from the research data.

Sustainable Recovery of Anthocyanins and Other Polyphenols from Red Cabbage Byproducts.

The objective of this work was to develop a sustainable process for the extraction of anthocyanins from red cabbage byproducts using, for the first time, apple vinegar in extractant composition. Our results showed that the mixture 50% (v/v) ethanol-water, acidified with apple vinegar, used in the proportion of 25 g of red cabbage by-products per 100 mL of solvent, was the best solvent for the preparation of an anthocyanin extract with good stability for food applications. The chemical characterization of this extract was performed by FTIR, UV-VIS, HPLC-DAD, and ICP-OES. The stability was evaluated by determining the dynamics of the total polyphenol content (TPC) and the total monomeric anthocyanin pigment content (TAC) during storage. On the basis of the statistical method for analysis of variance (ANOVA), the standard deviation between subsamples and the repeatability standard deviation were determined. The detection limit of the stability test of TPC was 3.68 mg GAE/100 g DW and that of TAC was 0.79 mg Cyd-3-Glu/100 g DW. The red cabbage extract has high TPC and TAC, good stability, and significant application potential. The extracted residues, depleted of anthocyanins and polyphenols with potential allelopathic risks, fulfill the requirements for a fertilizing product and could be used for soil treatment.

Solvent-Assisted Laser Desorption Flexible Microtube Plasma Mass Spectrometry for Direct Analysis of Dried Samples on Paper.

The present study investigated the potential for solvent-assisted laser desorption coupled with flexible microtube plasma ionization mass spectrometry (SALD-FμTP-MS) as a rapid analytical technique for direct analysis of surface-deposited samples. Paper was used as the demonstrative substrate, and an infrared hand-held laser was employed for sample desorption, aiming to explore cost-effective sampling and analysis methods. SALD-FμTP-MS offers several advantages, particularly for biofluid analysis, including affordability, the ability to analyze low sample volumes (<10 μL), expanded chemical coverage, sample and substrate stability, and in situ analysis and high throughput potential. The optimization process involved exploring the use of viscous solvents with high boiling points as liquid matrices. This approach aimed to enhance desorption and ionization efficiencies. Ethylene glycol (EG) was identified as a suitable solvent, which not only improved sensitivity but also ensured substrate stability during analysis. Furthermore, the addition of cosolvents such as acetonitrile/water (1:1) and ethyl acetate further enhanced sensitivity and reproducibility for a standard solution containing amphetamine, imazalil, and cholesterol. Optimized conditions for reproducible and sensitive analysis were determined as 1000 ms of laser exposure time using a 1 μL solvent mixture of 60% EG and 40% acetonitrile (ACN)/water (1:1). A mixture of 60% EG and 40% ACN/water (1:1) resulted in signal enhancements and relative standard deviations of 12, 20, and 13% for the evaluated standards, respectively. The applicability of SALD-FμTP-MS was further evaluated by successfully analyzing food, water, and biological samples, highlighting the potential of SALD-FμTP-MS analysis, particularly for thermolabile and polarity diverse compounds.

Malachite green dye adsorption from wastewater using pine gum-based hydrogel: Kinetic and thermodynamic studies

In this study, a novel Pn-g-poly(AAm) hydrogel was synthesized via free radical polymerization, using pine gum as the backbone material and polyacrylamide as the monomer. By employing response surface methodology and central composite design, various process parameters were optimized, achieving an optimum 1325 % maximum swelling. The optimized quantities were 0.085 g of initiator, 1.4 g of monomer, 0.013 g of crosslinker, and 14 ml of solvent. The physio-chemical characterizations were conducted using XRD, FE-SEM, FTIR, BET, and TGA. BET analysis showed a specific surface area of 34.973 m²/g and a pore volume of 0.104 cc/g. In adsorption studies, the highest removal (97 %) of malachite green (MG) dye was observed at pH 7, a temperature of 25 °C, a contact time of 5 h and 30 min, an adsorbent dose of 0.08 g, a dye concentration of 50 mg/L, and a shaking speed of 150 rpm. The adsorption data followed pseudo-second-order kinetics and Langmuir isotherm models, with a maximum adsorption capacity of 120.772 mg g−1. Furthermore, thermodynamic studies yielded ΔH° at 106.123 KJ/mol and ΔS° at 382.618 J/mol. These results collectively demonstrate the potential of this adsorbent for effectively treating industrial wastewater pollutants.

Hybrid ceramic nanofiltration membranes prepared by impregnation and solid-state grafting of organo-phosphonic acids

Grafting of oligomers into the mesopores of ceramic membranes (e.g. γ-alumina) represents an attractive strategy for deploying durable, resistant, and efficient hybrid membranes for the industrial treatment of wastewater containing organic solvents and divers solutes. In general, to control the membrane/solute/solvent interactions, homogeneous surface modification and high grafting yields are required. However, reaching this goal is rather challenging with the current grafting approaches where the active diffusion of the oligomers to the membrane pore surface may be hampered. To mitigate such diffusion limitation, we present here a novel synthesis method consisting of an infiltration of concentrated PEG organophosphonic acid oligomer solution in ceramic ultrafiltration membranes before initiating the solid-state grafting reaction to form a PEG-brush-grafted nanofiltration ceramic membrane. The infiltration step was found to be decisive for the formation of weak bonds between the oligomer linking functions and the ceramic membrane ensuring the final synthesis of robust PEG-based membranes by a grafting reaction. The influence of the solvent polarity (water vs. cyclohexane) on the conformation of the grafted PEG brush inside the γ-alumina mesopores was observed as a key parameter in the analysis of the pore size and permeability results. In addition to this, it was studied here for the first time by molecular dynamic simulations. The as-prepared PEG-brush/ceramic membranes were found very efficient in the separation of small organic dyes such as Rhodamine B (479 g mol−1) up to 85%. As a result, the present synthesis method represents a sustainable and simple alternative way for the preparation of hybrid nanofiltration membranes with controlled surface properties and attractive separation performance. Moreover, the vacuum impregnation and solid-state grafting approach requires a minimal amount of functional oligomers and solvent (0.5 mmol for 2–3 mL of solvent) and can be applied to other porous materials used in separation technologies.

Cyclodextrins Propolis Extract Encapsulation: Physicochemical Characterization, Toxicity Effect, and Application on Animal Sperm Cold Preservation

AbstractPropolis is composed of several bioactive compounds, which give it many beneficial biological effects. The use of cyclodextrins (CDs) is necessary when aiming to enhance the stability, absorption, and solubility of these substances in physiological media. The purpose of the present work is to study solubility diagrams of propolis extract of Melbou region (PEM) in the presence of CDs: α‐CD, β‐CD, and PM‐βCD, then to formulate an optimized preparation of the inclusion complex using a D‐optimal experimental design with three factors (ratio, ethanol solvent, and temperature). The optimal formulation is characterized by infrared spectroscopy (FTIR), X‐ray diffraction (XRD), and scanning electron microscopy (SEM). The cytotoxic and protective effects of the optimal formulation are evaluated in vitro against human red blood cells (RBCs) and beef sperm. The results show that PM‐βCD is more efficient, this is confirmed with an optimal formulation that obtained using 40 mL of solvent, a temperature of 40 °C with 1:1 stoichiometry. The cytotoxicity tests revealed that PEM and its inclusion complex are non‐toxic to RBCs and can maintain sperm conservation. It is concluded that PM‐βCD is more suitable to improve the solubility and stability of PEM constituents, and their non‐toxic effect has been approved.

Bioactive compounds recovery by freeze concentration process from winemaking by-product

Grape pomace is the main solid residue of wine industry, containing high amounts of phenolic compounds. Considering its high potential, an extraction procedure was optimized for maximal recovery of anthocyanins from grape pomace (Vitis vinifera L.) using citric acid as a generally recognized as safe (GRAS) acidulant in water. Volume of solvent (3.2–36.8 mL), time (14.4–165.6 min) and pH of solvent (1.12–4.48) were the studied variables. Furthermore, the best condition to obtain extract rich in anthocyanins was submitted to the gravitational block freeze concentration process. The performance of the process was evaluated and cryoconcentrated and ice fractions were analyzed for physicochemical properties, bioactive compounds content, and antioxidant activity. Interaction, linear, and quadratic effects for volume and pH of solvent were significant by analysis of variance (ANOVA). The experimental design allowed the prediction for maximal recovery of anthocyanins (10 mL of solvent at pH 1.8). The bioactive composition of the optimized grape pomace extract was influenced by the cryoconcentration process. After three cycles using gravitational block freeze concentration, the total phenolics and monomeric anthocyanins were approximately 4 and 5 times higher than the initial condition of the extract, respectively. Consequently, an increase in antioxidant activity was observed. The increase in the concentration of bioactive compounds reached a process efficiency of 93% (stage 1) for phenolic compounds and 91% (stage 2) for anthocyanins. Therefore, the final water-based optimized method is safe and has a low cost and the concentrated extract certainly showed higher concentrations of total phenolics and anthocyanins, compared to the initial extract. The proposed clean extraction method and cryoconcentration technique can be considered important strategies for recovering and valuing grape pomace components, improving the approach to the circular economy concept in the wine industry.

Roxadustat promotes hypoxia-inducible factor-1α/vascular endothelial growth factor signalling to enhance random skin flap survival in rats.

Random skin flaps have limited clinical application as a broad surgical reconstruction treatment because of distal necrosis. The prolyl hydroxylase domain-containing protein inhibitor roxadustat (RXD) enhances angiogenesis and reduces oxidative stress and inflammation. This study explored the function of RXD in the survival of random skin flaps. Thirty-six male Sprague-Dawley rats were randomly divided into low-dose RXD group (L-RXD group, 10 mg/kg/2 day), high-dose RXD group (H-RXD group, 25 mg/kg/2 day), and control group (1 mL of solvent, 1:9 DMSO:corn oil). The proportion of surviving flaps was determined on day 7 after surgery. Angiogenesis was assessed by lead oxide/gelatin angiography, and microcirculation blood perfusion was evaluated by laser Doppler flow imaging. Specimens in zone II were obtained, and the contents of superoxide dismutase (SOD) and malondialdehyde (MDA) were measured as indicators of oxidative stress. Histopathological status was evaluated with haematoxylin and eosin staining. The levels of hypoxia-inducible factor-1α (HIF-1α), vascular endothelial growth factor (VEGF), and the inflammatory factors interleukin (IL)-1β, IL-6, and tumour necrosis factor-α (TNF-α) were detected by immunohistochemistry. RXD promoted flap survival and microcirculatory blood perfusion. Angiogenesis was detected distinctly in the experimental group. SOD activity increased and the MDA level decreased in the experimental group. Immunohistochemistry indicated that the expression levels of HIF-1α and VEGF were increased while the levels of IL-6, IL-1β, and TNF-α were decreased after RXD injection. RXD promoted random flap survival by reinforcing vascular hyperplasia and decreasing inflammation and ischaemia-reperfusion injury.

Minimally Invasive Liquid Microjunction Sampling to Identify Dye on a 17th Century Spanish Illuminated Manuscript.

Common sampling methods for mass spectrometry such as sectioning are undesirably damaging to cultural heritage objects. A liquid microjunction sampling technique is developed that uses minimal solvent volume for analysis. Painted illustrations on a 17th century parchment manuscript from Spain were analyzed to identify the organic red pigment throughout its pages. By extracting with 0.1 μL solvent, the pigment was supplied for direct infusion electrospray MS, and the resulting disruption to the object surface was practically invisible to the naked eye.