Separations

This work reports the effect of scaling up annular centrifugal contactors (ACCs) upon the residence time distribution and the efficiency of extraction of uranium. The experiments were carried out in a multi-scale ACC platform of three ACCs with rotor diameters of 12, 25, and 40 mm. To enable direct comparison across all three scales of ACC, the residence time distributions were acquired by injecting dye into the solvent phase at a constant relative volume related to the ACC liquid holdup. Across all scales and flowrates, there was little difference in residence time distribution (<6 residence volumes), except for the smallest 12 mm rotor diameter ACC with a high solvent/aqueous feed ratio, which required 12 residence volumes, potentially due to internal circulation in the annulus. At low flowrates, the stage efficiency in all cases was >95%, and it improved further in larger rotor diameter ACCs. Full article

Tepotinib (MSC2156119) is a potent mesenchymal–epithelial transition (MET) factor inhibitor, a receptor tyrosine kinase that plays a crucial role in promoting cancer cell malignant progression. Adverse effects of tepotinib (TEP), such as peripheral edema, interstitial lung disease, nausea and diarrhea, occur due to drug accumulation and lead to termination of therapy. Therefore, the in silico and experimental metabolic susceptibility of TEP was investigated. In the current work, an LC-MS/MS analytical method was developed for TEP estimation with metabolic stability assessment. TEP and lapatinib (LTP) used as internal standards (ISs) were separated on a reversed-phase C18 column using the isocratic mobile phase. Protein precipitation steps were used to extract TEP from the human liver microsome (HLM) matrix. An electrospray ionization multi-reaction monitoring (MRM) acquisition was conducted at m/z 493→112 for TEP, at m/z 581→350, and 581→365 for the IS. Calibration was in the range of 5 to 500 ng/mL (R² = 0.999). The limit of detection (LOD) was 0.4759 ng/mL, whereas the limit of quantification (LOQ) was 1.4421 ng/mL. The reproducibility of the developed analytical method (inter- and intra-day precision and accuracy) was within 4.39%. The metabolic stability of TEP in HLM was successfully assessed using the LC-MS/MS method. The metabolic stability assessment of TEP showed intermediate Cl_int (35.79 mL/min/kg) and a moderate in vitro t_1/2 (22.65 min), proposing the good bioavailability and moderate extraction ratio of TEP. The in silico results revealed that the N-methyl piperidine group is the main reason of TEP metabolic lability. The in silico Star Drop software program could be used in an effective protocol to confirm and propose the practical in vitro metabolic experiments to spare resources and time, especially during the first stages for designing new drugs. The established analytical method is considered the first LC-MS/MS method for TEP estimation in the HLM matrix with its application to metabolic stability assessment. Full article

Artemisia negrei (A. negrei) and Artemisia aragonensis (A. aragonensis) are in the family Asteraceae, which has been used in traditional medicine. The use of plant-derived insecticides has become a promising strategy to reduce the harmful effects of synthetic insecticides and overcome the bio-resistance of pest insects to insecticides. In this regard, the purpose of the current study was to determine the chemical composition and evaluate insecticidal effects of essential oils (EOs) extracted from A. negrei (EON) and A. aragonensis (EOA). Notably, all chemical constituents present in the EOs were identified through GC-MS analysis, whilst the insecticidal properties against Callosobruchus maculatus Fab. (C. maculatus) were investigated by use of in vitro an in silico approaches. The obtained results showed that both tested EOs present a significant insecticidal effect against C. maculatus, which increased significantly upon the dose used in both contact and inhalation tests. The lethal concentrations (LC₅₀) for the inhalation test were found to be 2.1 and 2.97 μL/L, while in the contact test they were 2.08 and 2.74 μL/L of air for EON and EOA, respectively. At 5 μL/L of air, the spawn reduction rate was 88.53 % and 77.41%, while the emergence reduction rate was 94.86% and 81.22% by EON and EOA, respectively. With increasing doses of up to 20 μL/L of air, the reduction in individual emergence reached 100% by the two oils tested after 36 h of treatment. In addition, Molecular docking (MD) simulations supported the in vitro findings and indicated that certain identified components in EOA and EON exhibited stronger hydrogen bonding interactions with the target receptors. Interestingly, the prediction of ADMET properties indicates that the molecules investigated have great pharmacokinetic profiles with no side effects. Taken together, our findings suggest that EOA and EON may exert both potential contact and inhalation insecticidal actions and could be used as an alternative tool for the control of this major insect pest of stored products. Full article

Lithium silicate (LS) crack repairing material, working as a crystal waterproof material, could be used to strengthen concrete made from solid waste materials. This paper presents the results of water absorption and rapid freeze–thaw tests with concrete specimens coated with LS. Concrete specimens with different water–binder ratios and air content (0.35–1 and 0.55–4.5) were tested. The moisture uptake and water absorption coefficient were analyzed in the water absorption test. The water absorption coefficient of LS-coated specimens was lower than that of uncoated specimens, resulting in a lower total moisture content. The relative dynamic modulus of elasticity was calculated by the fundamental transverse frequency (Er) and ultrasonic velocity (Ev), respectively. Er and Ev exhibited similar attenuation characteristics, and the attenuation of LS-coated specimens was lower than that of uncoated specimens. A two-segment freeze–thaw damage model based on Er and Ev was employed to predict the service life of concrete. The relative errors of the service life results calculated by Er and Ev were within 10%. The two-segment freeze–thaw model could be used for the service life prediction of concrete structures. The present work provides new insight into using LS to improve the service life of concrete. Full article

Molecularly imprinted polymers are prepared in the presence of a template. They have been shown to resolve enantiomers when used as stationary phases for liquid chromatography. However, the separation efficiency is not as good as that observed with silica stationary phases. This manuscript identifies the main problems as the slow transfer kinetics between the mobile and stationary phase and the heterogeneity of the stationary phase binding sites. It suggests that preparing templated polymers that have predominantly or exclusively noncovalent crosslinks is the most promising approach for improving efficiency. Full article

The Moroccan picholine tree’s leaves contain phenolic compounds that benefit human health. However, the amount and type of these compounds can vary based on factors such as the extraction method and conditions. This study aimed to improve phenolic compounds’ extraction while minimising harmful chemicals’ use. It has been found that using ethanol as a solvent with ultrasonic extraction is the most effective and environmentally friendly technique. Several parameters, such as the extraction time, solid/solvent ratio, and ethanol concentration as independent variables, were evaluated using a surface response method (RSM) based on the Box–Behnken design (BBD) to optimize the extraction conditions. The experimental data were fitted to a second-order polynomial equation using multiple regression analysis and also examined using the appropriate statistical methods. In optimal conditions, the ultrasonic time, the ratio (solvent/solid) and the concentration (ethanol/water), the content of total polyphenols (TPC), total flavonoids (TFC), and antioxidant activity (by DPPH, ABTS, FRAP) were, respectively, 74.45 ± 1.22 mg EAG/g DM, 17.08 ± 1.85 mg EC/g DM, 83.45 ± 0.89% 82.85 ± 1.52%, and 85.01 ± 2.35%. The identification of phenolic compounds by chromatography coupled with mass spectrum (HPLC-MS) under optimal conditions with two successive extractions showed the presence of hydroxytyrosol, catechin, caffeic acid, vanillin, naringin, oleuropein, quercetin, and kaempferol at high concentrations. Full article

This work presents a sustainable and rapid method for halogenated pesticide analysis without chromatographic separation. The system is composed of a microfluidic open interface (MOI) for solid-phase microextraction (SPME) liquid phase desorption, connected to a liquid electron ionization mass spectrometry interface (LEI-MS). Either a triple quadrupole mass spectrometer (QQQ-MS/MS, (low-resolution) or a quadrupole-time-of-flight tandem MS (QTOF-MS/MS, high-resolution) were employed, each operating in negative chemical ionization (NCI) conditions. The flow rate used (100 µL/min) to rapidly empty the MOI chamber (approximately 2.5 µL) is reduced to the working flow rate of the LEI interface (500 nL/min) by a passive flow splitter (PFS). NCI is an appropriate ionization technique for electrophilic compounds, increasing specificity and reducing background noise. Two halogenated pesticides, dicamba and tefluthrin, were extracted simultaneously from a commercial formulation matrix (CF) using a C18 fiber by direct immersion (3 min under vortex agitation). Analyte desorption occurred in static conditions inside MOI filled with acidified acetonitrile (ACN) (0.2% phosphoric acid, PA). Extraction and desorption steps were optimized to increase efficiency and accelerate the process. No chromatographic separation was involved; therefore, the system fully exploited MS/MS selectivity and HRMS accuracy demonstrating good linearity, repeatability and limits of detection (LODs) and limits of quantification (LOQs) in the pg/mL range (50 and 500 pg/mL, respectively). Low-resolution experiments showed that matrix effects (ME) did not affect the results. The fast workflow (5 min) makes the system suitable for high-throughput analysis observing the principles of green analytical chemistry (GAC). Full article

Hyperhidrosis is a condition characterized by excessive sweating that affects at least 5% of the world’s population. It is normally associated with unpleasant body odour which requires continuous maintenance throughout life. Antiperspirants and deodorants are the first-line treatments for hyperhidrosis. However, association of this class of product with the risk of other diseases has increased the search for an effective antiperspirant from natural sources. This study aimed to investigate the antibacterial and antiperspirant activities of Curcuma xanthorrhiza Roxb. Using an in vitro microbial assay against specific bacteria responsible for body odour and rat foot pad analysis. Quality control of the fractionated extract was conducted using reversed-phase HPLC based on two active markers: xanthorrhiza and curcumin. Toxicity tests were conducted based on the OECD guidelines (50–2000 mg/kg). Inhibition zone, MIC, and MBC values of the hexane fraction of C. xanthorrhiza showed equivalent antibacterial activity to positive control (p > 0.05). No swelling, redness, or rashes were observed at the injection area throughout the study. Treatment with 40, 80, and 160 mg/kg of the extract significantly decreased the sweat excretion up to 79.34% (p < 0.05) after 15 min compared to negative control. Histopathology analysis showed the reduced size of the secretory units in plantar sweat glands post treatment compared to negative control. In conclusion, the hexane fraction of C. xanthorrhiza is able to reduce sweat excretion in a rat model and inhibit the growth of bacteria causing body odour. Full article

Chinese prickly ash and cinnamon contain many antioxidants, which scavenge free radicals and can reduce many harmful compounds, such as heterocyclic aromatic amines (HAAs). Modern technologies used for cooking, such as the use of superheated steam roasting, are beneficial in decreasing the development of HAAs. The current study was based on the use of these two spices in roasted lamb patties to mitigate the formation of HAAs in superheated steam roasted patties. Results exhibited significant differences (p < 0.05) in the content of both polar and non-polar HAAs as compared to control patties. In cinnamon roasted patties, polar HAAs were reduced from 23.76 to 10.56 ng g⁻¹, and non-polar HAAs were reduced from 21.34 to 15.47 ng g⁻¹. In Chinese prickly ash patties, polar and non-polar HAAs were 43.60 ng g⁻¹ and 35.74 ng g⁻¹, respectively. Similarly, cinnamon-treated patties showed a significantly higher (p < 0.05) reduction in polar HAAs (23.52 to 12.41 ng g⁻¹) than non-polar (16.08 to 9.51 ng g⁻¹) at concentrations of 0.5–1.5%, respectively, as compared to the control, with 45.81 ng g⁻¹ polar and 35.09 ng g⁻¹ non-polar HAAs. The polar HAAs tested were PhIP, DMIP, IQx, and 8-MeIQx, while the non-polar were harman and norharman. Both spices and superheated steam controlled HAAs to a significant level in lamb meat patties. Full article

Environmental adulteration is an emerging concern due to the discharge of wastewater effluents from several sources. Several carcinogenic dyes are the major contaminants in these water bodies. These could cause long-lasting and detrimental effects to humans as well as aquatic ecosystems. For efficient degradation of such dyes, the exploration of nanotechnology has demonstrated huge potential. Herein, the degradation of dyes (MB, CV, and MO) has been carried out photocatalytically using N-doped SnO₂ nanoparticles (N:SnO₂ NPs) as well as in presence of a sacrificial agent, EDTA. These NPs were synthesized at an ambient temperature. Different characterization techniques were used throughout the analysis of the synthesized NPs. The PXRD analysis reveals formation of single-phase rutile structure with tetragonal symmetry. Using the Scherrer formula, the size of the NPs was found to be less than 5 nm, exhibiting increases in size with N doping. Further, morphological analysis through field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) examined the existence of highly agglomerated, spherical NPs. The thermogravimetric analysis (TGA) results depict the thermal stability of the synthesized NPs up to a temperature of 800 °C. These synthesized N:SnO₂ NPs exhibit potent efficiency for the photocatalytic degradation of MB, MO, and CV dyes with an efficiency of 93%, 83%, and 73% degradation, respectively, under UV light irradiation. Additionally, the effect of the sacrificial agent, EDTA, was observed on the degradation process and resulted in a degradation of ~90% MB dye, 88% CV dye, and 86% MO dye within 15 min of UV light irradiation. Full article

Azo dyes such as Congo red can easily cause cancer when they come into contact or are absorbed by the human body, so it is urgent to find a fast and simple method for degrading Congo red. In order to better achieve this research goal, an ultrasonic method was used to degrade Congo red solution in a rotating flow field. The concentration of hydroxyl radical in the solution was significantly increased under the action of ultrasonic cavitation, chemical action of zero valent iron, and mechanochemistry. Under the strong oxidation of hydroxyl radical and the reduction of nano zero valent iron peeled off in the reaction process, the reaction speed is significantly accelerated and should promote the reaction. The effect of increasing stirring and adding iron powder particles on ultrasonic cavitation was studied by numerical simulation, and the yield of hydroxyl radical in the system was measured by fluorescence analysis. The experimental results show that, first, the rotating field formed by mixing increases the uniformity of ultrasonic sound field distribution and the amplitude of sound pressure, and it improves the cavitation intensity. In the effective dispersion area, the strong ultrasonic wave can form a temporary high-energy microenvironment in the suspension through cavitation, generate high strength shockwaves and micro jets, and thus significantly deagglomerate the iron powder aggregates. The addition of iron powder particles then provides a complementary Fenton reagent for the degradation reaction. The concentration of hydroxyl radicals in the solution was significantly increased by the synergy of the two actions. The degradation rate of Congo red reached more than 99% after 30 min of reaction. Full article

Capillary zone electrophoresis (CZE) is an important technique for the analysis of monoclonal antibodies (mAbs). A recently released light-emitting diode (LED)-induced fluorescence (LEDIF) detector equipped with a 275 nm LED for the detection of proteins through their native fluorescence was used in this study and compared to results obtained using the predominant detection mode, the measurement of the absorption of ultraviolet light (UV detection). This was accomplished using an established CZE method for the analysis of three mAbs: NISTmAb, matuzumab, and Intact Mass Check Standard (Waters). For this purpose, the detector’s settings were first optimized using a design of experiments approach. Three factors, rise time, photomultiplier high voltage supply, and acquisition frequency, were optimized by means of a D-optimal design. The optimal settings were then used for the investigation of signal-to-noise ratios (S/Ns), linearity, and precision. LEDIF detection offered a similar separation quality, up to 12 times higher S/Ns, and lower limits of detection compared to UV detection. Repeatability was excellent, with relative standard deviations (RSDs) of approximately 1% for percentage areas. For intermediate precision, RSDs of <2% (n = 3 × 10) were typically achieved. Overall, LEDIF detection was found to be an excellent and easily optimizable alternative to UV detection. Full article

This paper presents a numerical study of a closed-cycle evaporation system for the desalination of seawater. The system couples the condensing end of a heat pump with a humidifier, where the air is dehumidified in the heat pump evaporator. First, the mechanism of action of the closed-cycle evaporation system was analyzed from the perspective of heat transfer, and the control equations for the heat and mass transfer of the system were investigated. In addition, a mathematical model of the system was developed and validated. The influence of several important parameters of the air and seawater entering the system on the system’s performance under the design conditions was investigated numerically. The parametric analysis showed that the effect of the seawater mass flow rate on the system’s productivity was not significant. As the air mass flow rate increases, the freshwater production rate increases and then decreases. The output ratio (GOR) of the system was estimated and found to be competitive with other reported HDH systems. Full article

Background: Analytical techniques are a crucial method used in quality control procedures. Fusidic acid (FU), an antibacterial drug, is available on the market in a semisolid dosage form. This work aimed to develop a simple, sensitive, and robust UPLC assay for FU. Method: The effect of the formic acid concentration (X1 (1%, 0.55%, and 0.1%)), and column temperature (X2 (40, 32.5, and 25 °C)) on the retention time, peak area, and peak height were determined. Results: The results show that a long retention time of 1.18 min can be achieved with a low column temperature and a low to medium concentration of formic acid. A good peak height resolution was obtained with a low concentration of formic acid at different temperature settings. The optimized condition was suggested by the software program to analyze the drug in a mobile phase, consisting of 72% acetonitrile and 28% water containing 0.1% formic acid with a column temperature adjusted to 40 °C. Conclusion: The method was validated in terms of linearity, accuracy, precision, and robustness. In addition, the stability degradation study determined that the method can separate the drug from other degradation production. The method was applicable to determine the drug content in the marketed product. Full article

Membrane technology is an advanced hydrogen separation method that is of great significance in achieving hydrogen economy. Rare earth tungstate membranes have both high hydrogen permeability and remarkable mechanical/chemical stability, exhibiting good application prospects in hydrogen separation. This review provides the basic aspects and research progress on rare earth tungstate hydrogen separation membranes. The crystal structure, proton transport properties, and membrane stability under a chemical atmosphere are introduced. Different membrane construction designs, such as single-phase, dual-phase, and asymmetric rare earth tungstate membranes, are summarized. Lastly, the existing problems and development suggestions for tungstate membranes are discussed. Full article

In recent years, much attention has been paid to pharmaceuticals as potential toxic bioactive substances in the worldwide environment. These compounds are continuously introduced into the surroundings in small concentrations, which certainly affects the quality of water, ecosystem, and the general health of living organisms. Photocatalysis is a promising technique for treating pharmaceutically active compounds as organic pollutants over traditional technologies. This study proposes the application of photocatalysts composed of zinc oxide (ZnO) and tin oxide (SnO₂), synthesized using a solid-state method, for the photocatalytic degradation of two selected psychoactive drugs, amitriptyline (AMI) and alprazolam (ALP), under simulated solar and UV irradiation in an aqueous system. The newly synthesized photocatalysts were characterized using the following techniques: SEM/EDS, XRD, DLS, and UV/Vis spectroscopy. The obtained data confirmed the successful synthesis and the possible photocatalytic application of the new materials. Concerning the photocatalytic evaluation, the main results indicate that the highest removal efficiency of AMI and ALP was reached in the presence of ZnO/SnO₂ synthesized in a molar ratio of 2:1 and calcined at 700 °C, under 1.0 mg/mL catalyst loading. Based on the reutilization findings, it can be concluded that the mentioned photocatalyst had not lost its efficiency after three successive runs for the photodegradation of ALP. Additionally, pure ZnO powders showed the highest activity after calcination at 500 °C, in the case of both examined pollutants. The experiments with tert-butanol, sodium fluoride, and ethylenediaminetetraacetic acid suggested that the relative contribution of various reactive species changed in the following order: positively charged holes > ${\mathrm{OH}}_{\mathrm{free}}^{•}$ > ${\mathrm{OH}}_{\mathrm{ads}}^{•}$. Full article

Untargeted metabolomics approaches require complex samples containing the endogenous metabolites of a biological system. Here, we describe a set of protocols that can be applied to various types of samples, including prokaryotic and eukaryotic cells, as well as animal and human samples. Following a single extraction step, samples are analysed using different chromatographic conditions coupled to high-resolution mass spectrometry. Quantification of metabolite changes between samples is performed without internal standards, using peak areas from extracted ion chromatograms for statistical analysis. Bioinformatics annotation of the results allows a pathway- and process-oriented analysis across biological sample conditions, allowing a complete pathway interrogation. Full article

Phenolic compounds are important secondary metabolites often found in nature, and most prominently in plants. Plant biomass residues can be a sustainable source of this high-added-value group of compounds that can be used in the food and cosmetics industries due to their antioxidant properties. Olea europaea is a widely studied source of phenolic compounds, with olive leaves being an untapped solid residue with high phenolic content. Coffee residues after coffee extraction is another biomass residue stream rich in phenols. In this work, phenolic extracts of these two substrates, alongside different fractions produced through ultrafiltration and nanofiltration, were examined in resin adsorption experiments. Amberlite XAD16N was used as adsorbent in both batch and packed column experiments, with the experimental results being fitted with mathematical models for batch kinetics, adsorption isotherms, and column adsorption. The tested adsorbent proved capable of separating the target compounds, exhibiting a capacity of 72 mg of olive leaf phenols from nanofiltration retentate per g of resin in batch adsorption experiments, second order kinetics better described the batch adsorption process, while the use of the Thomas model sufficiently described the continuous adsorption process in packed columns (R² > 0.9). Full article