Separations, Volume 9, Issue 10 (October 2022) – 61 articles

Mixotrophic denitrification has showed great potential for treating wastewater with a low C/N ratio. Mixotrophic denitrification is the process combining autotrophic denitrification and heterotrophic denitrification in one system. It can compensate the disadvantage of the both denitrifications. Instead of using sodium acetate and glucose as carbon source for the heterotrophic denitrification, agriculture solid wastes including rice straw (RS), wheat straw (WS), and corncob (CC) were employed in this study to investigate their potential as carbon source for treating low C/N wastewater. The carbon releasing pattern of the three carbon rich materials has been studied as well as their capacity in denitrification. The results showed that the highest denitrification occurred in the corncob system which was 0.34 kg N/(m³·d). Corncob was then selected to combine with sulfur beads to build the mixotrophic denitrification system. The reactor packed with sulfur bead on the top and corncob on the bottom achieved 0.34 kg N/(m³·d) denitrification efficiency, which is higher than that of the reactor packed with completely mixed sulfur bead and corncob. The autotrophic denitrification and heterotrophic denitrification were 42.2% and 57.8%, respectively. The microorganisms in the sulfur layer were Thermomonas, Ferritrophicum, Thiobacillus belonging to autotrophic denitrification bacteria. Kouleothrix and Geothrix were mostly found in the corncob layer, which have the function for fiber hydrolysis and denitrification. The study has provided an insight into agriculture solid waste application and enhancement on denitrification of wastewater treatment. Full article

Given the increasing risks that antibiotic abuse poses to microecology and human health, it is imperative to develop incredibly powerful adsorbents. This study investigated the use of environmentally sustainable polymeric nanocomposite based on gum arabic (GA) and magnetic nanoparticles (MNPs) synthesized via co-precipitation method to form gum arabic magnetitic nanoparticles (GA-MNPs) as an efficient adsorbent for ciprofloxacin (CIP) removal from aqueous solution. The physicochemical properties and morphology of the synthesized GA-MNPs were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and Energy Dispersive X-Ray Analysis (EDX). The experiment was designed by response surface methodology (RSM) and the Central Composite Design (CCD) was utilized to optimize the operating variables: contact time (0–120 min), pH (3–10), adsorbent dosage (0.10–0.40 g/L), and concentration of adsorbate (5–100 mg/L). Results showed that 96.30% was the maximum percentage of CIP removed. The adsorption effect of the CIP molecule on the surface of the GA-MNPs was investigated using regression analysis and analysis of variance. Furthermore, Freundlich Isotherm and Pseudo Second order kinetic equations have the highest consistency with experimental investigations suggesting double-layer adsorption. This implies that chemisorption was the mechanism involved. In addition, the calculated thermodynamic parameters were postulating an exothermic and spontaneous method in nature. Owing to its adsorption selectivity and recyclability, GA-MNPs could be classified as an environmentally friendly, less expensive, and highly efficient promising adsorbent for remediation of CIP from aqueous solution. Full article

Blackberry is widely used in diets for its rich biological phytochemicals and health benefits. However, the relationship between the effect of blackberry extract (BBE) on ameliorating alcoholic liver disease (ALD) and the PXR-Cytochrome P450s axis in vivo and in vitro is unknown. In this study, 50% and 30% ethanol by gavage were used to establish acute and subacute ALD. Male mice were intragastrically administered BBE with 25, 50, and 100 mg/kg BW in the treatment groups. In the experiment, samples were collected, and related indices and histopathological observation were measured. In addition, the potential mechanism was predicted by network and docking studies, which were verified by qRT-PCR analysis, the detection of apoptosis, the measurement of mitochondrial membrane potential, the detection of ROS levels, and Western blotting in liver tissues and HepG2 cells. The acute and subacute ALD experiments indicated BBE ameliorated liver indices, AST, ALT, SOD, and MDA in serum, and the histopathology changed, as observed via H&E, Sirius red, and oil red O staining. The potential mechanism was predicted by network and docking studies, which were verified by experiments. Western blotting suggested BBE reduced the protein expression of NF-κB, TGF-β, IL-6, and α-SMA, and enhanced PXR and CAR in livers. In addition, qRT-PCR showed BBE significantly elevated the mRNA levels of PXR, CAR, CYP3A25, CYP3A11, and CYP2B10. In the experiment of the ethanol-induced apoptosis of HepG2 cells, BBE reduced the apoptosis of HepG2 cells by boosting mitochondrial membrane potential, reducing the apoptotic rate and ROS content, lessening the expression of Bax, and inducing the expression of PXR. For the first time, this study demonstrated BBE’s preventive effects on ALD, which are associated with the antioxidation and stimulation of the PXR-Cytochrome P450s axis. In addition, BBE is available as a nutritional agent. Full article

The synergistic effect of electrostatically enhanced fibrous filtration originates from the charging characteristics of aerosol particles and electret fibers in an electric field. Two electrostatically enhanced fibrous filter systems are designed in this study to investigate the mechanism of the effects of the charging characteristics of oily aerosol on the filtration efficiency. We investigate the charging characteristics and their effects on the filtration efficiency of dioctyl-phthalate (DOP) aerosol particles of various sizes by setting different filter systems and electric field intensities. The experimental results show that the charge of DOP particles increases with the strength of the electric field, and the average charge increases with the particle size. The maximum charge of DOP particles reaches 4760 eC/P, and the filtration efficiency of the coupled system improves when DOP particles are amply charged. For 0.25 μm DOP particles as the most penetrating particle size, the system had good long-term stability, and the filtration efficiency is approximately 72% higher than that of the fiber acting alone. Meanwhile, the problem of oily aerosol deposition reducing the electret filtration efficiency is solved, providing a basis for long-term filtration and oily aerosol purification by electret fiber. Full article

Vegetables and fruits can potentially accumulate cyanotoxins after water contaminated with cyanobacteria is used for irrigation. We developed and validated an analytical method to quantify eight microcystin congeners (MCs) and nodularin (NOD) using ultra high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) in three different matrices. Strawberries, carrots and lettuce are selected as model matrices to represent the fruits/berries, leafy and root vegetables, sequentially. The validation of a UHPLC-MS/MS method in the strawberry matrix is novel. Matrix effects are observed in all three matrices. Our methodology uses matrix-matched calibration curves to compensate for the matrix effect. The implementation of our method on 103 samples, containing nine different sorts of fruits and vegetables from the Belgian market, showed no presence of MCs or NOD. However, the recoveries of our quality controls showed the effectiveness of our method, illustrating that the use of this method in future research or monitoring as well as in official food controls in fruit and vegetable matrices is valid. Full article

The fragrance industry plays a key role in the global economy, producing a wide range of personal care and household products. However, some fragrance ingredients have been linked to allergic reactions in sensitive people, and their concentrations are regulated at the European level. For this reason, reliable, rapid, and sustainable analytical methods are needed to rapidly detect and quantify these compounds. Recently, a new class of hydrophobic eutectic solvents (HES) has been introduced; they consist of natural terpenoids or phenolic compounds that can be used as hydrogen bond donors (HBD) and acceptors (HBA), and they are more suitable for GC applications due to their higher volatility. In this study, a dispersive liquid–liquid microextraction (DLLME) approach is proposed for the analysis and quantification of a range of allergens in hydroalcoholic perfumes. The optimized method requires only 50 µL of a natural HES (thymol–eugenol), which is readily dispersed by vortexing in 2 mL of sample. After centrifugation, the HES rich phase is diluted in 400 µL EtOH and directly injected into the GC-FID system. The proposed method has been successfully applied in the analysis and quantification of commercial fragrances, demonstrating good enrichment of target allergens and suitability for aqueous matrices analysis. Full article

Tecoma stans is an ornamental perennial tropical and subtropical plant belonging to the Bignoniaceae family with green leaves and yellow attractive fragrance flowers and commonly known as yellow trumpetbush or yellow bells. The plant originated in the tropical areas of South America and Mexico and has been cultivated in many countries such as Egypt, Iraq, and the United Arab Emirates (UAE). T. stans has been found in different parts of the UAE such as Ras Al Khaimah, Abu Dhabi, and Dubai, where it can be seen in public parks, side roads, and home gardens. The Flash Chromatography System is used in different aspects of drug discovery studies because of its ability to purify secondary metabolites from crude plant extracts. A method was developed using the Flash Chromatography System to isolate three components from the ethanolic extract of T. stans leaves that showed in vitro antioxidant activity. In vitro evaluation of the antioxidant activity of the isolated components of T. stans was conducted using 1,1-diphenyl-2-picryl hydrazyl and 2, 2′-azinobis-3-ethylbenzothiazoline-6-sulfonic acid methods. Isolated components A-4, A-3, and A-2 had antioxidant activity when compared to ascorbic acid. Component A-3 showed antioxidant activity using the DPPH and ABTS methods; antifungal activities when tested against Candida albicans; and more than 80% inhibitions in the third dilution when compared to itraconazole and nystatin as positive controls. This rapid and efficient method using flash chromatography was used for the isolation and purification of an isolated component A-3 that showed both antioxidant and antifungal activities. Full article

Intensive greenhouse agriculture annually produces large amounts of residues. The present work focused on the study of the dynamic adsorption of cobalt from aqueous solutions over a vegetal residue from intensive greenhouse cultivation. The influence of three operating variables, feed-flow rate, inlet concentration of cobalt and bed height, was analyzed. According to the results, the variable that particularly affected the percentage of cobalt adsorbed was the feed-flow rate. The results were also fitted to an adaptive neuro fuzzy system (ANFIS) model to predict cobalt adsorption from aqueous solutions and choose the most favorable operating conditions. Results were evaluated using root mean squared error (RMSE), coefficient of determination (R2) and other typical statistic factors as performance parameters. The experimental and model outputs displayed acceptable result for ANFIS, providing R² values higher than 0.999 for both cobalt removal (%) and biosorption capacity (mg/g). In addition, the results showed that the best operating conditions to maximize the removal of cobalt were 4 mL/min of feed-flow rate, 25 mg/L of inlet concentration and 11.5 cm of bed-height. Full article

A novel BiOI/TiO₂ nano-heterojunction was prepared using hydrothermal and sol-gel methods. The composite material was characterized by X-ray diffraction, ultraviolet-visible diffuse reflection spectroscopy, scanning electron microscopy, and transmission electron microscopy. The crystallinity and response to light of BiOI/TiO₂ were controlled by preparation conditions such as the optimal solvent condition and heat treatment temperature. The photocatalytic activity of the BiOI/TiO₂ catalyst was examined using benzene as a test molecule. The benzene degradation rate of the composite catalyst under visible light was enhanced compared to pure TiO₂, thus reaching 40% of the original benzene concentration, which increased further to >60% after surface acidification. The fluorescence spectra, light current, and electron paramagnetic resonance confirmed that the enhanced activity was attributed to carrier separation by the heterojunction. The acid sites and active chlorine of hydrochloric acidification offer a novel mechanism for photocatalytic reactions. Full article

Taraxacum kok-saghyz Rodin (TKS) is a potential edible resource plant that is rich in inulin, lipid, protein and other active ingredients. In this study, HS-SPME/GC–MS was used to analyze volatile compounds (VCs) and profile the fatty acids in TKS roots and leaves, and the results were compared with those from Taraxacum officinale (TO). A total of 105 and 107 VCs were detected in the leaves and roots of seven dandelion samples (three TKS and four TO), amongst which the main VCs were ethyl tetradecanoate, ethyl linolenate, ethyl linoleate, dihydroactinidiolide, ethyl palmitate, β-ionone, 3,5-octadien-2-one, β-ionone 5,6-epoxide, geranyl acetone, benzaldehyde, safranal, 2-Pentylfuran, farnesene and β-elemene. Linoleic acid and linolenic acid were the dominant fatty acids in seven dandelion samples, and the ratio of unsaturated to saturated fatty acids was larger than 4. Principal component analysis showed that the differences in VCs and fatty acid levels between different dandelion samples mainly came from different places of origin, while the differences between different varieties in the same place of origin was minor; i.e., the VCs and fatty acid levels of TKS and TO collected from the same place were basically similar. Full article

Humic acids (HAs) and fulvic acids (FAs) are naturally occurring compounds that influence the fate and transportation of various compounds in the soil. Although HAs and FAs have multiple uses, the reports about their sorbent potential for environmental pollutants are scanty and sparse. In this study, HA and FA, isolated from lignite samples from two mines in Greece, were studied as sorbent materials for three active compounds of plant protection products, namely glyphosate (herbicide), cypermethrin (pyrethroid insecticide), and azoxystrobin (fungicide). According to the results, both HA and FA are promising sorbent materials for these active compounds, with HA achieving better sorption for cypermethrin and azoxystrobin, while FA was found to be more efficient for glyphosate. Moreover, their performance was not compromised by other components commonly found in commercially available herbicides/insecticides/fungicides. In addition, no significant leaching of the sorbed compounds was recorded. Finally, the two materials achieved similar sorption efficiency of the compounds from lake water. Full article

Honey adulteration with cheap sweeteners such as corn syrup or invert syrup results in honey of lesser quality that can harm the objectives of both manufacturers and consumers. Therefore, there is a growing interest for the development of a fast and simple method for adulteration detection. In this work, near-infrared spectroscopy (NIR) was used for the detection of honey adulteration and changes in the physical and chemical properties of the prepared adulterations. Fifteen (15) acacia honey samples were adulterated with glucose syrup in a range from 10% to 90%. Raw and pre-processed NIR spectra of pure honey samples and prepared adulterations were subjected to Principal Component Analysis (PCA), Partial Least Squares (PLS) regression, and Artificial Neural Network (ANN) modeling. The results showed that PCA ensures distinct grouping of samples in pure honey samples, honey adulterations, and pure adulteration using NIR spectra after the Multiplicative Scatter Correction (MSC) method. Furthermore, PLS models developed for the prediction of the added adulterant amount, moisture content, and conductivity can be considered sufficient for screening based on RPD and RER values (1.7401 < RPD < 2.7601; 7.7128 < RER < 8.7157) (RPD of 2.7601; RER of 8.7157) and can be moderately used in practice. The R²_validation of the developed ANN models was greater than 0.86 for all outputs examined. Based on the obtained results, it can be concluded that NIR coupled with ANN modeling can be considered an efficient tool for honey adulteration quantification. Full article

The need to get uranium out of leaching liquid is pushing scientists to come up with new sorbents. This study uses the wet technique to improve the U(VI) sorption properties of ZrO₂/chitosan composite sorbent. To validate the synthesis of ZrO₂/CS composite with Zirconyl-OH, -NH, and -NH₂ for U(VI) binding, XRD, FTIR, SEM, EDX, and BET are used to describe the ZrO₂/chitosan wholly formed. To get El Sela leaching liquid, it used 150 g/L H₂SO₄, 1:4 S:L ratio, 200 rpm agitation speed, four hours of leaching period, and particle size 149–100 µm. In a batch study, the sorption parameters are evaluated at pH 3.5, 50 min of sorbing time, 50 mL of leaching liquid (200 mg/L U(VI)), and 25 °C. The sorption capability is 175 mg/g. Reusing ZrO₂/CS for seven cycles with a slight drop in performance is highly efficient, with U(VI) desorption using 0.8 M acid and 75 min of desorption time. The selective U(VI) recovery from El Sela leachate was made possible using ZrO₂/CS. Sodium diuranate was precipitated and yielded a yellow cake with a purity level of 94.88%. Full article

The objective of this study was to develop and validate a near-infrared (NIR) spectroscopy based method for in-line quantification during the second alcohol precipitation process of Astragali radix. In total, 22 calibration experiments were carefully arranged using a Box–Behnken design. Variations in the raw materials, critical process parameters, and environmental temperature were all included in the experimental design. Two independent validation sets were built for method evaluation. Validation set 1 was used for optimization. Different spectral pretreatments were compared using a “trial-and-error” approach. To reduce the calculation times, the full-factorial design was applied to determine the potential optimal combinations. Then, the best parameters for the pretreatment algorithms were compared and selected. Partial least squares (PLS) regression models were obtained with low complexity and good predictive performance. Validation set 2 was used for a thorough validation of the NIR spectroscopy method. Based on the same validation set, traditional chemometric validation and validation using accuracy profiles were conducted and compared. Conventional chemometric parameters were used to obtain the overall predictive capability of the established models; however, these parameters were insufficient for pharmaceutical regulatory requirements. Then, the method was fully validated according to the ICH Q2(R1) guideline and using the accuracy profile approach, which enabled visual and reliable representation of the future performances of the analytical method. The developed method was able to determine content ranges of 8.44–39.8% at 0.541–2.26 mg/mL, 0.118–0.502 mg/mL, 0.220–0.940 mg/mL, 0.106–0.167 mg/mL, 0.484–0.879 mg/mL, and 0.137–0.320 mg/mL for total solid, calycosin glucoside, formononetin glucoside, 9, 10-dimethoxypterocarpan glucopyranoside, 2′-dihydroxy -3′, 4′-dimethoxyisoflavan glucopyranoside, astragloside II, and astragloside IV, respectively. These ranges were specific to the early and middle stages of the second alcohol precipitation process. The method was confirmed to be capable of achieving an in-line prediction with a very acceptable accuracy. The present study demonstrates that accuracy profiles offer a potential approach for the standardization of NIR spectroscopy method validation for traditional Chinese medicines (TCMs). Full article

We evaluated the potential use of agri-food waste for the removal of heavy metal ions from aqueous solutions and its application in different processes (e.g., water remediation, in the production of biomass enriched in nutritionally significant elements, etc.). Biomasses from grape seed, grape pomace, loquat seed, Calabrese broccoli stem, empty pods of carob and broad bean pods, unripe bitter orange peel, kumquat, orange pulp and Canary Island banana pulp were prepared. The percentages and biosorption capacities were evaluated and compared with those refe-renced using Valencia orange peel (Citrus sinensis Valencia late). These studies allow for easily providing added value to different agri-food wastes. The results show that the proposed biomasses were able to retain the studied metal ions and obtained different percentages, being in some cases above 90%. The highest values were obtained using broad bean pod (Pb(II) (91.5%), Cd(II) (61.7%), Co(II) (40.7%) and Ni(II) (39.7%)). Similar values were observed using grape seed, broccoli stem, carob pod and unripe bitter orange peel. Carob pod for biosorption of Cd(II) is also of great interest. These studies suggest that the agri-food residues evaluated can be applied to prepare effective biosorbents of divalent metal ions from aqueous solutions. Full article

A study of the plants, and their associated poisons, in the Poison Garden at The Alnwick Garden was undertaken across a calendar year. By selecting 25 plants in the Poison Garden, we have been able to develop a single chromatographic method for the determination and quantification of 15 plant toxins by liquid chromatography mass spectrometry (LC-MS). Chromatographic separation was achieved on a C18 column (3.5 µm, 100 × 4.6 mm) with a gradient method using water +0.1% formic acid and methanol +0.1% formic acid. The developed method was validated for precision, linearity, limits of detection and quantification and extraction recoveries. The method showed good linearity with a R² value of >0.995 for all 15 compounds with good precision of 10.7%, 6.7% and 0.3% for the low, medium and high calibration points, respectively. The LC-MS method was used to analyse 25 plant species, as well as their respective parts (i.e., bulb, flower, fruit, leaf, pollen, seed, stem and root), to assess the human risk assessment to children (aged 1 to <2 years) in relation to the plant toxin and its respective LD₅₀. The analysis found that the greatest potential health risks were due to the ingestion of Colchicum autumnale and Atropa belladonna. As a caution, all identified plants should be handled with care with additional precautionary steps to ensure nil contact by children because of the potential likelihood of hand-to-mouth ingestion. Full article

Nitrogen oxide (NOx) is a major gaseous pollutant in flue gases from power plants, industrial processes, and waste incineration that can have adverse impacts on the environment and human health. Many denitrification (de-NOx) technologies have been developed to reduce NOx emissions in the past several decades. This paper provides a review of the recent literature on NOx post-combustion purification methods with different reagents. From the perspective of changes in the valence of nitrogen (N), purification technologies against NOx in flue gas are classified into three approaches: oxidation, reduction, and adsorption/absorption. The removal processes, mechanisms, and influencing factors of each method are systematically reviewed. In addition, the main challenges and potential breakthroughs of each method are discussed in detail and possible directions for future research activities are proposed. This review provides a fundamental and systematic understanding of the mechanisms of denitrification from flue gas and can help researchers select high-performance and cost-effective methods. Full article

The title ligand (L^”_x), methyl 2-((4-cyanophenyl)(hydroxy)methyl)acrylate was synthesized following the Morita-Baylis-Hillman reaction scheme. Spectroscopic techniques such as: UV- Visible, FT-IR, ESI-MS, and ¹H NMR helped in characterization of the L^”_x. Complexes of Cr³⁺, Co³⁺, Ni²⁺, Mn²⁺, Cu²⁺ with L^”_x were prepared and characterized by UV- Visible, FT-IR and powder-XRD. FTIR spectrum of the L^”_x generated through DFT B3LYP method and 6-311++ G (d,p) basis set was found in good agreement with experimental spectrum. Additionally, the semi-empirical PM6 method optimization helped propose the most suitable geometries of the complexes with Cr³⁺, Co³⁺ possessing octahedral, Ni²⁺ square planner, Mn²⁺ and Cu²⁺ tetrahedral geometries. Powder-XRD patterns of the complexes have revealed cubic crystal class for Cr³⁺ and Co³⁺, whereas hexagonal, orthorhombic, and monoclinic for Ni²⁺, Mn^2+, and Cu²⁺ complexes were observed, respectively. In addition, the nano-particle size was found in the range of 8.2560–4.5316 nm for complexes. Antibacterial activity against S. aureus, E. coli, B. pumilis and S. typhi confirmed a substantially high potential, as endorsed by their Molecular docking studies, of Ni²⁺ and Cu²⁺ complexes against each bacterial strain. Moreover, all compounds exhibited positive antioxidant activities, but have no antifungal potential except L^”_x. The current study demonstrates the usefulness of these novel transition metal complexes as possible potent antibacterial and antioxidant agents. Full article

The periodic injection-production process of natural gas in underground gas storage make the rock bear alternating load under the gas-solid coupling. The alternating load changes the physical properties of rock, and then influence the critical production pressure drop of injection-production wells in gas storage. In the case of gas-solid coupling, the decisive factors affecting the alternating load are the number of injection-production cycles and the injection-production differential pressure. Therefore, a discrete element numerical simulation model is established to simulate the gas-solid coupling process of gas storage wells under different injection-production cycle and differential pressure. The influence mechanism of injection-production cycle and differential pressure on particle cementation and primary crack is analyzed microscopically and also the influence law of injection-production cycle and differential pressure on rock mechanical properties is analyzed from the macroscopic. Finally, the influence law of injection-production cycle and differential pressure on the critical production pressure drop of injection-production wells due to gas-solid coupling can be obtained. The results show that under the influence of gas-solid coupling, the number of bonded contact cracks and micro cracks in the model increase gradually, both the elastic modulus ratio and the cohesion ratio decrease gradually with the increase of injection-production cycle and the higher the injection-production differential pressure, the greater the decline range. Then, with the injection-production cycle increasing the Poisson’s ratio increases gradually and the higher the injection-production differential pressure, the greater the increase range. Finally, the internal friction angle ratio increases greatly in the initial stage, after that decreases and then shows a linear increase. According to the influence law, the relationship model between the critical production pressure drop of injection-production wells in gas storage and the injection-production cycle and differential pressure under the gas-solid coupling will be established, which is used for the dynamic prediction of the critical production pressure drop of injection-production wells in the whole life cycle of gas storage. Full article

Taxanes are natural compounds with strong antitumor activity. In this study, we first enriched taxanes by ultrasonic extraction and liquid–liquid extraction from Taxus cuspidata, then purified these taxanes by the antisolvent recrystallization method, and discussed the effects of four recrystallization conditions on the purity of eight target compounds. The most promising purification results were obtained using methanol as a solvent and water as an antisolvent. Response surface methodology (RSM) was used to further optimize the optimal purification conditions: when the crude extraction concentration was 555.28 mg/mL, an antisolvent to solvent volume ratio was 28.16 times, the deposition temperature was 22.91 °C, and the deposition time was 1.76 min, the purity of the taxanes reached its maximum. The scanning electron microscopy (SEM) results showed that recrystallization could effectively reduce the particle size of crude Taxus cuspidata and control the particle morphology. X-ray diffraction (XRD) and Raman spectrum experiments demonstrated that the amorphous state of the crude Taxus cuspidata did not change during the recrystallization process, and always remained amorphous. This recrystallization method can effectively improve the purity of taxanes in Taxus cuspidata, and is suitable for the preliminary purification of taxanes. Full article

A novel, sensitive, and low-cost HPLC method for the rapid determination of favipiravir (FVR) in rat plasma was developed and validated, and the effect of vitamin C on FVR pharmacokinetic parameters was investigated. FVR and oxcarbazepine (IS) were separated using a mobile phase of 50% acetonitrile and 50% water (with 0.25% trifluoroacetic acid) at 1.0 mL/min flow rate and detected at λmax 289 nm. The intra- and interday values for FVR in plasma were less than 15%, with low, medium, and high QC levels for the relative recovery rate, according to ICH guidelines. Cmax values in the control and experimental groups were 558 ± 124.42 and 979.13 ± 138.10 ng/mL, respectively; t_1/2 values were 7.15 ± 1.60 and 9.09 ± 1.14 h, AUC_(0-t) values were 5697.70 ± 536.58 and 7381.62 ± 1577.58 ng.h/mL, and AUC_(0-∞) values were 5697.70 ± 536.58 and 8192.36 ±  1721.67, respectively. According to the results, the experimental group’s Cmax of FVR was 75.17% higher than the control group’s, the Vz/F was lower, and the t_1/2 was 1.86 h longer. The technique developed for determining FVR in plasma was useful for FVR pharmacokinetics and food–drug interaction investigations. Full article

Pulsed electric field (PEF) is a sustainable innovative technology that allows for the recovery of nutrients and bioactive compounds from vegetable matrices. A. bisporus was chosen for its nutritional value and the effect of PEF pretreatment was evaluated using different conditions of electric field (2–3 kV/cm), specific energy (50–200 kJ/kg) and extraction time (0–6 h) to obtain the best conditions for nutrient and bioactive compound extraction. Spectrophotometric methods were used to evaluate the different compounds, along with an analysis of mineral content by inductively coupled plasma mass spectrometry (ICP-MS) and the surface was evaluated using scanning electron microscopy (SEM). In addition, the results were compared with those obtained by conventional extraction (under constant shaking without PEF pretreatment). After evaluating the extractions, the best extraction conditions were 2.5 kV/cm, 50 kJ/kg and 6 h which showed that PEF extraction increased the recovery of total phenolic compounds in 96.86%, carbohydrates in 105.28%, proteins in 11.29%, and minerals such as P, Mg, Fe and Se. These results indicate that PEF pretreatment is a promising sustainable technology to improve the extraction of compounds and minerals from mushrooms showing microporation on the surface, positioning them as a source of compounds of great nutritional interest. Full article

Several analytical methods are documented for the estimation of vitamin D3 (VD3) in pharmaceuticals, food supplements, nutritional supplements, and biological samples. However, greener analytical methods for VD3 analysis are scarce in the literature. As a consequence, attempts were made to design and validate a greener “high-performance thin-layer chromatography (HPTLC)” method for VD3 estimation in commercial pharmaceutical products, as compared to the traditional HPTLC method. The greenness indices of both approaches were predicted by utilizing the “Analytical GREENness (AGREE)” method. Both traditional and greener analytical methods were linear for VD3 estimation in the 50–600 ng band⁻¹ and 25–1200 ng band⁻¹ ranges, respectively. The greener HPTLC strategy outperformed the traditional HPTLC strategy for VD3 estimation in terms of sensitivity, accuracy, precision, and robustness. For VD3 estimation in commercial tablets A–D, the greener analytical strategy was better in terms of VD3 assay over the traditional analytical strategy. The AGREE index of the traditional and greener analytical strategies was estimated to be 0.47 and 0.87, respectively. The AGREE analytical outcomes suggested that the greener analytical strategy had a superior greener profile to the traditional analytical strategy. The greener HPTLC strategy was regarded as superior to the traditional HPTLC methodology based on a variety of validation factors and pharmaceutical assays. Full article

In the literature, greener/eco-friendly analytical techniques for simultaneous estimation of chlorzoxazone (CZN) and paracetamol (PCT) are scarce. As a consequence, greener reverse-phase high-performance thin-layer chromatography with ultraviolet (HPTLC-UV) detection was developed and validated for simultaneous estimation of CZN and PCT in commercial capsules and tablets. The greenness of the proposed HPTLC-UV technique was assessed quantitatively by utilizing the “Analytical GREENness (AGREE)” methodology. For simultaneous estimation of CZN and PCT, the greener HPTLC-UV technique was linear in the 40–1600 ng band⁻¹ and 30–1600 ng band⁻¹ ranges, respectively. Furthermore, the suggested HPTLC-UV methodology proved sensitive, accurate, precise, and robust for simultaneous detection of CZN and PCT. The assay of CZN in marketed capsules and tablets was found to be 99.01 ± 1.53 and 100.87 ± 1.61%, respectively, using the suggested HPTLC-UV method. The assay of PCT in commercial capsules and tablets was found to be 98.31 ± 1.38 and 101.21 ± 1.67%, respectively. The AGREE index for the greener HPTLC-UV technique was found to be 0.79, suggesting an excellent greenness profile for the proposed HPTLC-UV technique. These results and data suggested the suitability of the greener HPTLC-UV methodology for simultaneous estimation of CZN and PCT in commercial formulations. Full article

The objectives of this research were to carry out GC–MS and LC–MS-based phytochemical profiling of Barleria hochstetteri, as well as flow cytometry-based mechanistic investigations of the cytotoxic effect of its extracts against breast and lung cancer cell lines. This preclinical in vitro study was carried out in Saudi Arabia and India, from 11 August to 15 January 2022. Barleria hochstetteri was sequentially extracted using the Soxhlet extraction technique. Utilizing LC–MS and GC–MS methods, the phytochemical profiling was performed. Additionally, the total phenolic compounds and flavonoids were quantified in the plant extract using spectrophotometric techniques. In this study, we first examined the cytotoxicity of the plant extract on non-malignant L929 cells and on the carcinogenic MCF-7 and A549 cell lines. Then, we studied the underlying molecular pathways by means of Anti-Bcl-2, caspase-3, and DNA fragmentation (TUNEL) assays, using flow cytometry. The results revealed phenolic compounds and flavonoids to be the two major components in the methanolic extract of B. hochstetteri, with concentrations of 3210 µg GAE/g dwt and 1863 µg QE/g dwt, respectively. Results from GC–MS and LC–MS analyses revealed the presence of bioactive phytochemicals with known cytotoxicity. From the MTT assay on cell viability, the IC₅₀ of the methanol extract for the MCF-7 and A549 cell lines were 219.67 and 144.30 µg/mL, respectively. With IC₅₀ values of 324.24 and 266.66 µg/mL, respectively, the aqueous and methanol extracts were less toxic when tested against the non-cancerous L929 cell line. The extract caused early and late apoptosis in the tested breast and lung cancer cells by activating caspase-3 and inhibiting Bcl-2 protein, and it also caused cell death via DNA damage, based on flow cytometric and molecular marker analyses. These findings indicate that the methanol extract of B. hochstetteri was cytotoxic on breast cancer and lung cancer cell lines. To uncover cancer-fighting chemicals, there is a need for further research on B. hochstetteri, as it is a promising source of anti-cancer chemotherapeutic drugs. Full article

Oxytropis microphylla (Pall.) DC. is a traditional Tibetan medicine used as an external preparation for clearing heat and detoxification, healing sore muscles, astringent vein hemostasis, defecation, and treating plague, constipation, anthrax, and swollen and painful furuncles. It remains a challenge to comprehensively analyze and identify the chemical constituents of Oxytropis microphylla (Pall.) DC. In this study, a new analytical method using a combination of ultra-high-performance liquid chromatography–mass spectrometry (UHPLC-MS) and effective data mining techniques was established to identify the chemical constituents of Oxytropis microphylla. A total of 127 compounds were identified in O. microphylla extract, including 92 flavonoids, 15 indole alkaloids, and 20 others. After the oral administration of the extract to rats, 22 metabolites were identified in the plasma. The primary in vivo metabolic reactions that occurred after the administration of O. microphylla extract were glucuronidation and sulfation. Therefore, we successfully devised a high-efficiency method to distinguish compounds and used it as a source of post-study to identify the active biological components of O. microphylla extract. Full article

The chestnut postharvest pathogen Neofusicoccum parvum (N. parvum) is an important postharvest pathogen that causes chestnut rot. Chestnut rot in postharvest reduces food quality and causes huge economic losses. This study aimed to evaluate the inhibitory effect of dill seed essential oil (DSEO) on N. parvum and its mechanism of action. The chemical characterization of DSEO by gas chromatography/mass spectrometry (GC/MS) showed that the main components of DSEO were apiole, carvone, dihydrocarvone, and limonene. DSEO inhibited the growth of mycelium in a dose-dependent manner. The antifungal effects are associated with destroying the fungal cell wall (cytoskeleton) and cell membrane. In addition, DSEO can induce oxidative damage and intracellular redox imbalance to damage cell function. Transcriptomics analysis showed DSEO treatment induced differently expressed genes most related to replication, transcription, translation, and lipid, DNA metabolic process. Furthermore, in vivo experiments showed that DSEO and DSEO emulsion can inhibit the growth of fungi and prolong the storage period of chestnuts. These results suggest that DSEO can be used as a potential antifungal preservative in food storage. Full article

This study analyses the concept of a novel multi-crystallization system to achieve zero liquid discharge (ZLD) for desalination plants using an innovative heat recovery system consisting of a heat transfer fluid and a compressor to reduce energy consumption. The main focus is to recover water and separately extract salts from seawater brines with high purity, including calcite, anhydrite, sodium chloride, and epsomite, which can be sold to the cement industry. The system is compared with a conventional brine treatment system. The energy demand and economic feasibility of both systems are assessed to evaluate profitability at a scale of 1000 kg/h. The results estimate that the utilization of a heat recovery fluid reduces energy consumption from 690 kWh_th/ton of feed brine to 125.90 kWh_th/ton equaling a total electric consumption of 60.72 kWh_e/ton. The system can recover 99.2% of water and reduce brine discharge mass by 98.9%. The system can recover 53.8% of calcite at near 100% purity, 96.4% of anhydrite at 97.7% purity, 91.6% of NaCl at near 100% purity, and 71.1% of epsomite at 40.7% purity. Resource recovery accounts for additional revenues, with halite and water accounting respectively for 69.85% and 29.52% of the income. The contribution of calcite and anhydrite to revenue is very low due to their low production. The levelized cost of water (LCOW) of the multi-crystallization system is 13.79 USD/m³ as opposed to 7.85 USD/m³ for the conventional ZLD system. The economic analyses estimate that the conventional ZLD system can achieve payback after 7.69 years. The high electricity cost, which accounts for 68.7% of the annual expenses, can be produced from renewable sources. Full article

Phthalates are widely used in industry, but adverse effects on human health have been reported due to exposure to these chemicals. In the human body, they are metabolized into phthalic monoesters, which are used to monitor human exposure and assess risk. Urine is one of the main biological samples used, due to its easy access and collection, and also being the main elimination pathway for phthalates. Urine samples are complex; therefore, sample preparation is a critical step. Disposable pipette extraction (DPX) has not previously been reported for quantifying phthalates in urine and is here presented as a fast and low sample consumption method. A fully optimized RP-DPX method was developed for determination of free monomethyl phthalate, monobutyl phthalate, monobenzyl phthalate, and monoethylhexyl phthalate from urine samples. Analytical parameters of merit were obtained. The values of R2 were ≥0.9832, and the LOD and LOQ varied from 3.0 to 7.6 μg L⁻¹ and 10 to 25 μg L⁻¹, respectively. Intraday (n = 3) and interday (n = 9) precision were ≤13.6 and 15.6%. The accuracy, as relative recovery, presented a range from 83 to 120%. The method was robust after performing the Youden test. Compared to other methods, this work stands out due to its short extraction time and sample consumption. Full article