Dichloromethane Research Articles

Determination of Patulin in Apple Juice and Apple-Derived Products Using a Robotic Sample Preparation System and LC-APCI-MS/MS.

Patulin, a toxic mycotoxin, can contaminate apple-derived products. The FDA has established an action level of 50 ppb (ng/g) for patulin in apple juice and apple juice products. To effectively monitor this mycotoxin, there is a need for adequate analytical methods that can reliably and efficiently determine patulin levels. In this work, we developed an automated sample preparation workflow followed by liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI-MS/MS) detection to identify and quantify patulin in a single method, further expanding testing capabilities for monitoring patulin in foods compared to traditional optical methods. Using a robotic sample preparation system, apple juice, apple cider, apple puree, apple-based baby food, applesauce, fruit rolls, and fruit jam were fortified with 13C-patulin and extracted using dichloromethane (DCM) without human intervention, followed by an LC-APCI-MS/MS analysis in negative ionization mode. The method achieved a limit of quantification of 4.0 ng/g and linearity ranging from 2 to 1000 ng/mL (r2 > 0.99). Quantitation was performed with isotope dilution using 13C-patulin as an internal standard and solvent calibration standards. Average recoveries (relative standard deviations, RSD%) in seven spike matrices were 95% (9%) at 10 ng/g, 110% (5%) at 50 ng/g, 101% (7%) at 200 ng/g, and 104% (4%) at 1000 ng/g (n = 28). The ranges of within-matrix and between-matrix variability (RSD) were 3-8% and 4-9%, respectively. In incurred samples, the identity of patulin was further confirmed with a comparison of the information-dependent acquisition-enhanced product ion (IDA-EPI) MS/MS spectra to a reference standard. The metrological traceability of the patulin measurements in an incurred apple cider (21.1 ± 8.0 µg/g) and apple juice concentrate (56.6 ± 15.6 µg/g) was established using a certified reference material and calibration data to demonstrate data confidence intervals (k = 2, 95% confidence interval).

Synthesis, characterisation and voltammetric study of dimethylammonium lead iodide perovskite

In the last decade, the most investigated perovskite materials are the hybrid organic-inorganic perovskites (HOIPs) due to their optoelectronic properties and possible application in the production of photovoltaics. This interest has led to an ongoing search for new HOIP variants, alongside thorough investigations of the properties of existing HOIPs. That is why our research in the field of organic-inorganic perovskites is aimed at the synthesis, characterization, and investigation of the electrochemical properties of dimethylammonium lead iodide (DMAPbI3) using voltammetric studies. A modified synthesis of DMAPbI3, differing slightly from the one described in the literature, was performed by combining stoichiometric amounts of lead iodide (PbI2) and dimethylammonium iodide (DMAI) dissolved in acetonitrile. After conducting controlled evaporation, a yellow crystalline powder of DMAPbI3 was obtained. The identity and purity of the obtained compound were confirmed by powder X-ray diffraction (PXRD), infrared (IR) and Raman spectroscopy, and scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX). Investigations on the electrochemical properties of DMAPbI3 by cyclic voltammetry were performed with dichloromethane (DCM) and tetrabutylammonium chloride (TBAC) as the electrolyte. A paraffin-impregnated graphite electrode (PIGE) was used as a working electrode, on which the perovskite microparticles were immobilized. The electrochemical activity of DMAPbI3 is recognized through an intense, broad, and irreversible anodic peak attributed to the oxidation of the constituents to different possible products and the decomposition of the perovskite structure.

Functional Hydrogels Promote Vegetable Growth in Cadmium-Contaminated Soil.

Over the years, the concentration of cadmium in soil has increased due to industrialization. Cadmium in the soil enters the human body through plant accumulation, seriously endangering human health. In the current study, two types of hydrogels were successfully synthesized using a free radical polymerization method: an ion-type hydrogel referred to as DMAPAA (N-(3-(Dimethyl amino) propyl) acrylamide)/DMAPAAQ (N,N-Dimethyl amino propyl acrylamide, methyl chloride quaternary) and a non-ion-type hydrogel known as DMAA (N,N-Dimethylacrylamide). In the experiment carried out in this study, the ion-type hydrogel DMAPAA/DMAPAAQ was introduced to cadmium-contaminated soil for vegetable cultivation. The study found that at cadmium levels of 0 and 2 mg/kg in soil, when exposed to a pH 2 solution, cadmium wasn't detected in the filtrate using ICP. As the amount of cadmium increased to 500 mg/kg, hydrogel addition gradually reduced the filtrate cadmium concentration. Notably, the use of the 4% hydrogel resulted in 0 mg/L of cadmium. For the 0% hydrogel, vegetable cadmium absorption was determined to be 0.07 mg/g, contrasting with 0.03 mg/g for the 4% hydrogel. The DMAPAA/DMAPAAQ hydrogel significantly boosts vegetable growth by efficiently absorbing nitrate ions through ion exchange, releasing them for plant uptake. In contrast, the DMAA hydrogel, used as a control, does not enhance plant growth despite its water absorption properties. In summary, the composite hydrogel shows great potential for enhancing vegetable yield and immobilizing heavy metals in soil.

Antibiotic Activity of a Newly Discovered Aspergillus Species Isolated from Sewage Dump Site

Infectious agents causing diseases are becoming resistant to drugs produced to manage them. This has continued to spur scientific investigations for newer and better antibiotics to aid and/or replace existing ones. Soil samples were collected from sewage dump sites with the sole aim of isolating and screening fungi species for antibacterial substances using the cultural method. A newly discovered fungi species of Aspergillus was used to produce crude antibiotic, fractionated by column chromatography and tested on clinical isolates – Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae, Candida albicans and Pseudomonas aeruginosa. The result of zones of inhibition was 45 mm, 47 mm, 48 mm, 49 mm and 47 mm in order of listing of organisms. Gas chromatography mass spectrometry analysis of the fractionated extract revealed the following compounds as being responsible for the observed inhibition – methylene chloride, heptanoic acid, octanoic acid, methyl hydrogen phthalate, 2,4-di-tert-butylphenol, dodecanoic acid, z-10-tetradecen-1-ol acetate, tetradecanoic acid, 2-tetradecyloxy-ethanol, n-hexadecanoic acid, hexadecanamide, octadecenamide and octadecanamide. A cocktail of organic compounds – fatty acids and amides that displayed strong antimicrobial ability, if well tapped, hold a future in the development of new antibiotics.

Recovery of Chromium and Two Solvents (Dichloromethane-DCM Tetrachloroethane-TCE) Using Nanofiltration and Reverse Osmosis Membranes from Leather Industry Wastewater

In this study, for removal of the leather industry pollutants and to recovery of chromium (Cr), dichloromethane (DCM) and tetrachloroethane (TCE) two sequential nanofiltration (NF) (NF90 and NF270) and two reverse osmosis (RO) (BW30 and SW30) reactor membranes were used. The membrane surface properties were investigated by Fourier Transform Infrared Spectroscopy-Attenuated Total Reflectance (FTIR-ATR) and Scanning Electron Microscopy (SEM). The permeate of the SW30 reverse osmosis exhibited high removals varying between 98% and 99% for sodium ion (Na+ ), potassium ion (K+ ), magnesium ions (Mg2+), calcium ions (Ca2+), total chemical oxygen demand (CODtotal), dissolved chemical oxygen demand (CODdis), dissolved organic carbon (DOC) and inert chemical oxygen demand (inert COD), Chromium (Cr3+ ), Dichloromethane and Tetrachloroethane. In the NF90 nanofiltration process lower removals were detected (96%-97%) for all pollutants mentioned above. The effluent of reverse osmosis with a BW30 membrane match to the Turkish Water Pollution Control Regulation rules for treated water discharged to the receiving environment while SW30 reverse osmosis membrane was perfect for ultimate treatment of the pollutants present in the leather industry discharges. From the concentrate of the SW30 reverse osmosis, 945 mg/l chromium, 460 mg/l dichloromethane and 360 mg/l tetrachloroethane were reused. The performance and recoveries of Cr and two solvents (DCM and TCE) data in NF and RO membrane reactors were evaluated with Artificial Neural Network (ANN) process and Kruskal Wallis test statistic coupled with Mann-Whitney U statistic in this study.

Isolation of a Marker Olean-12-en-28-butanol Derivative from Viscum continuum E. Mey. Ex Sprague and the Evaluation of Its Antioxidant and Antimicrobial Potentials.

Viscum continuum E. Mey. Ex Sprague (Mistletoe) is a semi-parasitic plant that grows on the branches of other trees with reported numerous biological activities. This study was aimed at isolating a compound/s that will be used as a standard reference for quality control of South African-based commercialized mistletoe products and to further perform antioxidant and antimicrobial tests on the isolated compound. A dried sample of mistletoe was ground and extracted successively with hexane, dichloromethane (DCM), acetone and methanol using a serial exhaustive cold maceration procedure. The compound was isolated using column chromatography, and its chemical structure was elucidated using two-dimensional nuclear magnetic resonance (2D NMR) and ultrahigh-performance liquid chromatography-mass spectrometry (UPLC-MS). The antioxidant activity of the compound was determined using DPPH, hydrogen radical scavenging activity and reducing power assays, whereas antimicrobial activity was assessed using the minimum inhibitory concentration (MIC) method. Subjection of the DCM extract to column chromatography resulted in the isolation of a compound elucidated as olean-12-en-28-butanol-1-one, 3-hydroxy-4,4,10, 14, 20-pentamethyl (D4). Both the DPPH, H2O2 radical scavenging activity and reducing power assays revealed a significant antioxidant potential of compound D4 with an IC50 of 0.701 mg/mL, lower than that of gallic acid (0.793 mg/mL) for the H2O2 radical scavenging assay. The results also indicated good antibacterial activity of D4 with an IC50 of 0.25 mg/mL, compared to ciprofloxacin with an IC50 of 0.0039 mg/mL, against two Gram-negative (Pseudomonas aeruginosa, Escherichia coli) and three Gram-positive (Streptococcus pyogenes, Bacillus cereus and Staphylococcus aureus) bacteria. This study is the first to report on the isolation of the olean-12-en-28-butanol derivative from mistletoe of the South African ecotype.

Experimental and theoretical studies on effective synergistic low-temperature removal of NO and typical volatile organic compounds (VOCs) from flue gas based on Cu@VWTi catalyst

The transition metal-modified VWTi structural catalysts hold great promise for simultaneously removing nitrogen oxides (NOx) and volatile organic compounds (VOCs) from industrial flue gases. A series of Cu@VWTi catalysts were prepared to investigate their synergistic low-temperature removal performance towards NO and typical VOCs, including toluene, benzene, chlorobenzene (CB), p-chlorotoluene (p-CT), and dichloromethane (DCM). The copper-enhanced samples prepared via ultrasound-assisted impregnation exhibited irregular globular and varying crystallinity. The catalysts displayed a typical anatase crystal structure with high TiO2 content or high dispersion of V and W species along with a certain adjustment effect on the morphology. Various controlling factors affecting the synergistic removal of NO and VOCs were evaluated. It was observed that the presence of VOCs in flue gas has weak impact on NO removal, except for the waste incineration using the Cu@VWTi catalyst. However, a high initial NO concentration had an adverse effect on VOCs removal. Impressively, the optimized copper-doped catalyst (5 wt% Cu loaded of smelting plant and coal-fired power plant used catalyst) exhibited excellent performance for p-CT, toluene and DCM removal of 95.0%, 99.6% and 100% at 300 °C, respectively. The toluene and p-CT conversion efficiencies were highest over the catalyst used in the smelting plant after Cu loading, surpassing the benzene conversion efficiency. Cu@VWTi demonstrated excellent performance for p-CT, toluene, and DCM removal at 250 °C. Although 5 wt% Cu loading on the catalysts significantly enhanced the stability and anti-jamming of VOCs removal, as well as their tolerance to both SO2 and water vapor. The enhanced mechanism of Cu decoration attributed to the enhanced intensity of acid sites and the stable relative proportion of Oads/Olatt species in the used 5% Cu loaded catalyst due to the redox cycles of Cu and V species. Compared with Brønsted acid, which primarily adsorbs NH4+, Lewis acid mainly adsorbs gas phase acid and forms coordinated NH3 in gas phase. The bonding between toluene and the Cu site was enhanced with an adsorption energy of −130.9 kJ mol−1, as well as the cracking adsorption of the CH2Cl2 on the Ti site with a bonding energy of −436.7 kJ mol−1, both indicating strong chemical adsorption. The first step of dechlorination and demethylation was thermodynamically and kinetically favorable for DCM and toluene decomposition.

Phytochemical evaluation of Ziziphus mucronata and Xysmalobium undulutum towards the discovery and development of anti-malarial drugs

BackgroundThe development of resistance by Plasmodium falciparum is a burdening hazard that continues to undermine the strides made to alleviate malaria. As such, there is an increasing need to find new alternative strategies. This study evaluated and validated 2 medicinal plants used in traditional medicine to treat malaria.MethodsInspired by their ethnobotanical reputation of being effective against malaria, Ziziphus mucronata and Xysmalobium undulutum were collected and sequentially extracted using hexane (HEX), ethyl acetate (ETA), Dichloromethane (DCM) and methanol (MTL). The resulting crude extracts were screened for their anti-malarial and cytotoxic potential using the parasite lactate dehydrogenase (pLDH) and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay, respectively. This was followed by isolating the active compounds from the DCM extract of Z. mucronata using silica gel chromatography and structural elucidation using spectroscopic techniques (NMR: 1H, 12C, and DEPT). The active compounds were then targeted against P. falciparum heat shock protein 70–1 (PfHsp70-1) using Autodock Vina, followed by in vitro validation assays using ultraviolet–visible (UV–VIS) spectroscopy and the malate dehydrogenase (MDH) chaperone activity assay.ResultsThe extracts except those of methanol displayed anti-malarial potential with varying IC50 values, Z. mucronata HEX (11.69 ± 3.84 µg/mL), ETA (7.25 ± 1.41 µg/mL), DCM (5.49 ± 0.03 µg/mL), and X. undulutum HEX (4.9 ± 0.037 µg/mL), ETA (17.46 ± 0.024 µg/mL) and DCM (19.27 ± 0.492 µg/mL). The extracts exhibited minimal cytotoxicity except for the ETA and DCM of Z. mucronata with CC50 values of 10.96 and 10.01 µg/mL, respectively. Isolation and structural characterization of the active compounds from the DCM extracts revealed that betulinic acid (19.95 ± 1.53 µg/mL) and lupeol (7.56 ± 2.03 µg/mL) were responsible for the anti-malarial activity and had no considerable cytotoxicity (CC50 > µg/mL). Molecular docking suggested strong binding between PfHsp70-1, betulinic acid (− 6.8 kcal/mol), and lupeol (− 6.9 kcal/mol). Meanwhile, the in vitro validation assays revealed the disruption of the protein structural elements and chaperone function.ConclusionThis study proves that X undulutum and Z. mucronata have anti-malarial potential and that betulinic acid and lupeol are responsible for the activity seen on Z. mucronata. They also make a case for guided purification of new phytochemicals in the other extracts and support the notion of considering medicinal plants to discover new anti-malarials.

Separation and characterization of the antioxidant active component from Maillard reaction products in xylose-lysine system

ABSTRACT Maillard reaction products (MRPs) play a crucial role in preserving food quality due to their antioxidant capacity. In this study, we isolated and characterized the antioxidant components from MRPs using a xylose-lysine system under optimal conditions. Methylene chloride and ethyl acetate were employed for sequential extractions, and the ethyl acetate phase underwent thin-layer chromatography and silica column separation. The identified compound, 3-hydroxy-4-methyl-2(5 H)-furanone (3H4MFN), was analyzed using FT-IR, GC-MS, and NMR, revealing its volatile nature with a chemical formula of C5H6O3. Further activity analysis demonstrated that 3H4MFN exhibited higher or comparable antioxidant activity to vitamin C (VC) and vitamin B6 (VB6). This newly discovered compound shows potential as a natural antioxidant in cosmetics, food, and nutraceutical applications.

Structural and sound absorption properties of polyethylene terephthalate (PET) and recycled polyethylene terephthalate (r-PET) nanofibers

Sound-absorbing materials are used to reduce noise pollution since noise is one of the important environmental factors affecting human health. Due to their high porosity and large specific surface area, nanofibers can be preferred as a better sound absorption material. In this study, nanofiber-based sound-absorbing materials are produced using polyethylene terephthalate (PET) and recycled polyethylene terephthalate (r-PET) in the electrospinning method in order to obtain a thin and high-sound absorbing material. Another objective of this study is to investigate the performance of r-PET compared to PET from the sound absorbing properties points of view to contribute sustainability which is one of the most important issues of today. For these purposes, solutions of three different concentrations (10%, 15% and 20% owf) were prepared by dissolving PET and r-PET polymers in trifluoroacetic acid (TFA):dichloromethane (DCM) solvent mixture. It will also be possible to help sustainability issues by reducing environmental pollution and raw material costs by using r-PET. Samples were electrospun on a polypropylene based nonwoven structure using solutions at different flow rates (0.1-0.3-0.5 ml/h) and needle tip-collector distances (4–8 cm). The fiber diameter, thickness, bulk density, porosity and pore size properties of the produced samples were investigated. The sound absorption coefficient (SAC) was measured with a dual microphone impedance tube device. The relationship between the structural properties of the samples and the SAC was evaluated. SAC decreased with increasing fiber diameter, bulk density, pore size and increased with high porosity. These values were compared with different sound absorbing materials which are commonly used. According to the results, the developed nanofiber-based material with a 0.3 mm thickness has high SAC values compared to conventional sound absorbing materials with 10–16 mm thickness values, especially in middle frequency levels. Recycled polymer may be preferred when PET and r-PET nanofibers show similar results.

Unlocking the functional potential of Nitraria schoberi extracts using chemical fingerprinting, biological efficiencies, in silico and network pharmacological approaches

The objective of this investigation was to assess the cytotoxic, antioxidant, and enzyme inhibitory properties of the aerial portions of Nitraria schoberi (family Nitrariaceae). Extracts were prepared by sequential maceration in hexane, dichloromethane (DCM), ethyl acetate and methanol (MeOH) and water extract was prepared by infusion. DCM and MeOH extracts accumulated the highest amount of metabolites where the former was characterized by the presence of octadecyl ferulate (16.96 mg/100 mg), methoxyluteolin (8.48 mg/100 mg) and isorhamnetin (5.35 mg/100 mg) and the alkaloids perlolyrine (5.03 mg/100 mg), (+)-5a-hydroxylemannine (2.43 mg/100 mg) and matrine (2.40 mg/100 mg). Results of antioxidant activity showed that the MeOH extract exerted the highest anti-2,2-diphenyl-1-picrylhydrazyl (DPPH) (28.13 mg Trolox equivalent (TE)/g) and Fe+++ (54.38 mg TE/g) reducing capacity. All extracts exerted significant acetylcholinesterase (3.71–4.37 mg galantamine equivalent (GALAE)/g) and tyrosinase (86.40–109.63 mg kojic acid equivalent (KAE)/g) inhibition activity. The best α-amylase and α-glucosidase inhibition was exhibited by the DCM (0.81 mmol ACAE/g) and MeOH (1.34 mmol ACAE/g) extracts respectively. The highest cytotoxic effect was exerted against the breast adenocarcinoma (MDA-MB-231) (IC50: 26.71 μg/mL) and cervix adenocarcinoma (HELA) (IC50: 29.10 μg/mL) cell lines by the MeOH and DCM extracts respectively. In addition, we performed molecular docking analysis to understand the interaction between chemical components and tested enzymes and cellular targets for cancer. Chrysoeriol-3-O-rutinoside bound strongly to AChE. Furthermore, a good interaction between vascular endothelial growth factor receptor 2 (VEGFR2) and isovitexin-2″-O-arabinoside was observed. We employed network pharmacology to understand the role of N. schoberi's compounds in neurological disorder like Alzheimer and multiple sclerosis. Therefore, the results of this study indicate that N. schoberi may serve as a viable starting point for the future creation of phytopharmaceuticals that target particular diseases associated with oxidative stress, such as diabetes and certain neurological disorders.

Enhancing C[sbnd]Cl bond cleavage and ozone conversion: Optimizing surface Co3+ and chemosorbed oxygen through polystyrene and dodecylamine modification

The activation of CCl bonds and the conversion of O3 are crucial for the degradation of chlorinated hydrocarbons through catalytic ozonation. This work constructed the surface active sites of Co3O4 with polystyrene (PS) and dodecylamine to enhance dichloromethane (DCM) removal and O3 conversion in photo-ozone catalysis simultaneously. The dodecylamine created active Co3+ on the catalyst surface, and the PS prevented the elimination of active Co3+ during calcination by forming CCoO. The O3 pre-treatment removed the deposited carbon to expose the active Co3+ and the chemisorbed oxygen. The surface Co3+ played a crucial role in cleaving the CCl bonds of DCM, and the chemosorbed oxygen facilitated the conversion of O3 into O. Moreover, the photogenerated holes oxidized the intermediates formed after the DCM dechlorination. The removal rate of DCM for the sample co-modified by PS and dodecylamine was 80.8 mg/(g‧h) under one sun irradiation, which was 2.2 times higher than that by Co3O4.

Removal of Mo(VI), Pb(II), and Cu(II) from wastewater using electrospun cellulose acetate/chitosan biopolymer fibers

Environmentally friendly polymers such as cellulose acetate (CA) and chitosan (CS) were used to obtain electrospun fibers for Cu2+, Pb2+, and Mo6+ capture. The solvents dichloromethane (DCM) and dimethylformamide (DMF) allowed the development of a surface area of 148 m2 g−1 for CA fibers and 113 m2 g−1 for cellulose acetate/chitosan (CA/CS) fibers. The fibers were characterized by IR-DRIFT, SEM, TEM, CO2 sorption isotherms at 273 K, Hg porosimetry, TGA, stress-strain tests, and XPS. The CA/CS fibers had a higher adsorption capacity than CA fibers without affecting their physicochemical properties. The capture capacity reached 102 mg g−1 for Cu2+, 49.3 mg g−1 for Pb2+, and 13.1 mg g−1 for Mo6+. Furthermore, optimal pH, adsorption times qt, and C0 were studied for the evaluation of kinetic models and adsorption isotherms. Finally, a proposal for adsorbate-adsorbent interactions is presented as a possible capture mechanism where, in the case of Mo6+, a computational study is presented. The results demonstrate the potential to evaluate the fibers in tailings wastewater from copper mining.

EPA bans most uses of methylene chloride

EPA bans most uses of methylene chloride

Rational solvent selection for the preparation of industrial monolithic supported liquid-phase (SLP) olefin hydroformylation catalyst

Heterogenisation of the hydroformylation (HyFo) process converting C4 olefins and syngas (CO/H2) to n-pentanal can substantially reduce its carbon footprint by simplifying downstream processing. Current upscaling efforts include constructing a pilot plant containing a Rh-diphosphite-stabilized supported liquid-phase (SLP) catalyst. The air-sensitive nature of the catalyst requires in-situ impregnation of the porous support material with the liquid phase components (Rh-precursor, ligand, stabiliser) entailing the use of large quantities of an organic solvent. Environment, health, and safety (EHS) as well as regulatory aspects prompt the search for an alternative to dichloromethane (DCM), which was used as standard solvent for lab-scale studies. To obtain alternatives to DCM, the replacement solvent methyl tert-butyl ether (MTBE) and in-silico screening of more than 5000 solvent candidates has been performed covering boiling points and solubility predictions by COSMO-RS as well as carcinogenicity- and mutagenicity predictions by quantitative structure–activity relationship (QSAR) models. The final list of solvent candidates contained unsaturated compounds (alkenes, alkynes) in addition to ether- and ester-functionalized​ solvents, which are typically recommended as DCM replacements. Sufficiently high solubilities of ligand and stabiliser to prepare the desired SLP catalyst were experimentally determined in the following solvents: methyl propionate (MP), dimethoxymethane (DMM), MTBE, tetrahydrofuran (THF) and DCM for benchmarking, and a monolithic SLP catalyst prepared with MTBE demonstrated to perform equally well in the HyFo reaction of 1-butene as the benchmark catalyst prepared using DCM solvent. Overall, the study demonstrates a practical approach for selecting solvents with a greener profile for making catalyst systems applicable for large-scale production.

Development of Perfluoro Decalin/Fluorinated Polyimide Core-Shell Microparticles via SPG Membrane Emulsification Using Methyl Perfluoropropyl Ether Cosolvent.

Red blood cell-inspired perfluorocarbon-encapsulated core-shell particles have been developed for biomedical applications. Although the use of perfluorodecalin (FDC) is expected for core-shell particles owing to its high oxygen solubility, the low solubility of FDC in any organic solvent, owing to its fluorous properties, prevents its use in core-shell particles. In this study, a new cosolvent system composed of dichloromethane (DCM) and heptafluoropropyl methyl ether (HFPME) was found to dissolve both FDC and fluorinated polyimide (FPI) based on a systematic study using a phase diagram, achieving a homogeneous disperse phase for emulsification composed of oxygen-permeable FPI and oxygen-soluble FDC. Using this novel cosolvent system and Shirasu porous glass (SPG) membrane emulsification, FDC-encapsulated FPI shell microparticles were successfully prepared for the first time. In addition to oxygenation, demonstrated using hypoxia-responsive HeLa cells, the fabricated core-shell microparticles exhibited monodispersity, excellent stability, biocompatibility, and oxygen capacity.

Experimental investigation of PCL‐based composite material fabricated using solvent‐cast 3D printing process

AbstractBone tissue engineering relies on scaffolds with enhanced mechanical properties, achievable through 3D printing techniques. Our study focuses on enhancing mechanical properties using a solvent‐cast 3D printing method. For this, poly‐ε‐caprolactone (PCL) reinforced with polyhydroxybutyrate (PHB), and synthetic fluorapatite (FHAp) nanopowders were utilized, immersed in a solution of dichloromethane (DCM) and dimethylformamide (DMF). Sol–gel method was used to synthesized FHAp, and the XRD pattern confirmed crystalline FHAp presence, with notable peaks at 2θ values of 31.937°, 33.128°, 32.268°, and 25.864°. Moreover, composites exhibited nonchemical PCL‐PHB/FHAp interactions, with PHB and FHAp crystallographic planes evident. Surface roughness, assessed via RMS values, showed progressive increases with higher PHB and FHAp content. Tensile strength peaked at 19% wt/v of PHB, with varied effects of FHAp. Compressive strength reached its apex at 30% wt/v of FHAp, with higher PHB content consistently enhancing strength. Flexural strength notably increased with PHB, peaking at 19% wt/v, and further with FHAp. Young's modulus rose with both PHB and FHAp content. Hardness increased with PHB and FHAp, notably peaking at 30% wt/v of FHAp. Cell viability improved with PHB, showing varied responses to FHAp. Hemocompatibility evaluations indicated low hemolysis percentages, especially in balanced PHB/FHAp compositions. These findings highlight the crucial role of composite compositions in tailoring mechanical and biological properties for optimal bone scaffold design, promising advancements in tissue regeneration technologies.

Comparative antioxidant, antibacterial, and antidiabetic activities of in vitro-grown callus and wild-grown various parts of Piper longum L

BackgroundPiper longum L. is a tropical and subtropical medicinal plant that has been used as antidiabetic, diarrhea, stomachache, cough, asthma, and bronchitis since ancient times. The in vitro-grown callus from the leaf, however, has not been tested and utilized for any of these conditions. Thus, this research pursues to assess the comparative study of antioxidant, antibacterial, and antidiabetic activities of in vitro-grown callus and various parts of Piper longum-grown in the wild. MethodsThe antioxidant activity of crude extracts and the fractions were determined by DPPH (1,1-diphenyl-2-picrylhydrazyl) free-radical scavenging assay, the antibacterial activity by agar-well diffusion method, and antidiabetic activity by α-amylase and α-glucosidase inhibition assay. In addition, the total phenol content (TPC) and total flavonoid contents (TFC) were calculated using Folin-Ciocalteau reagent and aluminum chloride complex-forming assay respectively. ResultsThe highest antioxidant activity (IC50=134.81±1.16 µg/mL), TPC (41.22±0.50 mg of GAE/g dry weight), and TFC (73.41±0.53 mg of QE/g dry weight) were obtained in the dichloromethane (DCM) fraction of root than other crude extracts and fractions. The DCM fractions of root exhibited the minimum inhibitory concentration (MIC) at 5.0 mg/mL and minimum bactericidal concentration (MBC) of 8.35 mg/mL to the Staphylococcus aureus. Moreover, the DCM fraction of root showed the highest α-amylase and α-glucosidase inhibition (IC50=365.21±31.02 and 489.07±27.96 µg/mL) than other crude extracts and fractions. To the best of our information, comparative antioxidant (IC50=206.61±0.64 µg/mL), antibacterial (suppressed 80 % of tested bacteria), and antidiabetic (IC50=1165.15±15.63 and 1304.76±12.43 µg/mL) properties of the in vitro-grown callus were recorded for the first time in P. longum, and were found to be comparative to those of the wild-grown parts. ConclusionsThese results showed that wild-grown P. longum roots, particularly the DCM fraction, could be an important source of natural antioxidants, antimicrobials, and antidiabetics for better curative uses than other wild-grown parts and in vitro-grown callus. In vitro-grown callus, however, could be used as a natural drug source and used to conserve P. longum in its natural habitats in the future.

An eco-friendly and cost-effective HPTLC method for quantification of COVID-19 antiviral drug and co-administered medications in spiked human plasma

The coronavirus-2 has led to a global pandemic of COVID-19 with an outbreak of severe acute respiratory syndrome leading to worldwide quarantine measures and a rise in death rates. The objective of this study is to propose a green, sensitive, and selective densitometric method to simultaneously quantify remdesivir (REM) in the presence of the co-administered drug linezolid (LNZ) and rivaroxaban (RIV) in spiked human plasma. TLC silica gel aluminum plates 60 F254 were used as the stationary phase, and the mobile phase was composed of dichloromethane (DCM): acetone (8.5:1.5, v/v) with densitometric detection at 254 nm. Well-resolved peaks have been observed with retardation factors (Rf) of 0.23, 0.53, and 0.72 for REM, LNZ, and RIV, respectively. A validation study was conducted according to ICH Q2 (R1) Guidelines. The method was rectilinear over the concentration ranges of 0.2–5.5 μg/band, 0.2–4.5 μg/band and 0.1–3.0 μg/band for REM, LNZ and RIV, respectively. The sensitivities of REM, LIN, and RIV were outstanding, with quantitation limits of 128.8, 50.5, and 55.8 ng/band, respectively. The approach has shown outstanding recoveries ranging from 98.3 to 101.2% when applied to pharmaceutical formulations and spiked human plasma. The method’s greenness was assessed using Analytical Eco-scale, GAPI, and AGREE metrics.

Mapping the Influence of Solvent Composition over the Characteristics of Polylactic Acid Nanofibers Fabricated by Electrospinning

AbstractThis study investigated the solubility of poly(lactic acid) (PLA) in various solvents (to achieve an 8 % (w/v) polymer solution) and its impact on the morphology of electrospun PLA nanofibers. Several solvents, such as dichloromethane (DCM), chloroform (CHL), tetrahydrofuran (THF), acetone (AC), acetonitrile (ACTNR), dimethylformamide (DMF), dimethylacetamide (DMAc), ethylene glycol (ETGLY), distilled water (WATER), methanol (MEOH), formic acid (FA), and n‐hexane (NHX) were used in their pure and binary forms at several ratios (4 : 1, 2 : 1, 1 : 1, 1 : 2, 1 : 3, and 1 : 4). The study aims to explore the correlation between PLA solubility and its electrospinnability using solvents mapped from the Teas graph across different parameter zones and chemical groups. Hansen solubility parameters, including dispersion cohesion fractional solubility parameter (fd), the polar cohesion fractional solubility parameter (fp) was employed to identify the most effective solvents for PLA dissolution. Teas graph analysis highlighted a correlation between PLA solubility and solvent proximity to Hansen solubility parameters. Additionally, the solubility time varied between 1 hour and 24 hours. Polar solvents such as DCM, CHL, THF, ACTNR, and FA were able to dissolve 8 % (w/v) of PLA at different times, but only very high and effective dissolution of PLA was achieved in pure DCM and CHL whereas FA dissolved PLA in 24 hours, which resulted in the slowest solubility rate. Several structures of nanofibers, such as smooth, heterogenous, porous, fibrous, and beaded, were observed and discussed accordingly in terms of solvent type and ratio. The average nanofiber diameter ranged between 0.18 μm and 3.81 μm. Moreover, physical tests, including surface tension, density, viscosity, and conductivity, were conducted on solvent systems and CHL displayed higher viscosity, while ACTNR had the lowest viscosity and highest conductivity among pure solvents. According to the results of our study, it is possible to design further studies with the aim of deciding which solvents or binary forms should be applied to dissolve PLA within a certain time. The desired structure can be easily arranged to be used as a filter, biomimicking tissue environment, drug delivery system, or extra.