Methanol Water Research Articles

The Effect of Bacterial AHL on the Cyclic Adenosine Monophosphate Content in Plants According to High-Performance Liquid Chromatography.

Cyclic adenosine monophosphate (cAMP) is an important second messenger in cells, mediating various stimulation signals such as the growth and development of organisms and stress and participating in regulating various biological processes of cells. This article explores the quantitative determination of cAMP in plants using High-Performance Liquid Chromatography (HPLC) and applies this method to analyzing the changes in cAMP content during the process of plant response to the bacterial quorum sensing signal N-acyl homoserine lactone (AHL). Research has shown that the optimal detection conditions for HPLC are as follows: the chromatographic column is Venusil MP C18 (2), the mobile phase is methanol-water (0.1% trifluoroacetic acid) (v:v, 10:90), the detection wavelength is 259 nm, the column temperature is 35 °C, and the flow rate is 0.8 mL/min. The precision of the standard sample of this method is 98.21%, the precision of the sample is 98.87%, and the recovery rate is 101.067%. The optimal extraction conditions for cAMP in Arabidopsis are to use 15% methanol ultrasonic extraction for 10 min, followed by a 40 °C water bath for 4 h. Bacterial AHL signal processing can significantly stimulate an increase in cAMP levels in Arabidopsis leaves and roots. The establishment of HPLC detection methods for the cAMP content in plants is of great significance for in-depth research on the signal transduction mechanisms of plant-bacterial interactions.

Influence of Genotype on Antioxidant Activity and Phenolic Profile of Fennel Bulbs

Currently, fennel bulb is becoming a highly demanded and consumed vegetable due to its licorice flavor and health benefits. Although the chemical composition of fennel essential oil has been extensively studied, the nonvolatile bioactive compounds of fennel bulbs have drawn less attention. Here, the phenolic profile and the antioxidant activity in terms of DPPH radical scavenging activity, reducing power, chelating ability of ferrous ions, and inhibition of lipid peroxidation were analyzed using four different fennel hybrid genotypes and three different extraction solvents (methanol, aqueous-methanol, and hot water). Antioxidant activity results revealed significant variation amongst fennel varieties (>3-fold difference for DPPH and reducing power and >2.7-fold for the inhibition of lipid peroxidation), with methanolic extracts exhibiting the highest antioxidant activity. Total phenol content peaked in the aqueous-methanol extracts, exhibiting a 2-fold difference across fennel genotypes. HPLC–PDA/MS analyses identified high levels of caffeic acid derivatives in hot water extracts, particularly in the commercial genotype. The therapeutic benefits associated with these compounds make it reasonable to use detailed phytochemical screening in fennel breeding programs to obtain varieties with new functionalities and thus higher added value.

Experimental study on the effects of water addition in methanol on the performance of diesel-methanol diffusion combustion on a high-speed engine

Methanol is regarded as a low-carbon renewable fuel which is friendly to the environment. For purpose of investigating the impact of water introduction in methanol on diesel-methanol diffusion combustion, experimental tests were performed on a refitted dual-fuel high-speed diesel engine test bench. This research compared the differences between diesel-methanol diffusion combustion (DMDC) mode and diesel-hydrous methanol diffusion combustion (DHMDC) mode with a water mass content of 20%. The tests were performed by maintaining the engine speed of 3000 rpm and varying engine load as well as methanol injection timing (MIT). The results indicate that the heat release process in DHMDC mode begins later but is more rapid and concentrated compared to DMDC mode. The addition of 20% water in methanol does not significantly decreases the peak average in-cylinder temperature. However, it decreases the NOx emissions by up to approximately 40%. Water introduction leads to higher CO and THC emissions in DHMDC mode, but the retardation of MIT helps mitigate the increase in CO and THC emissions. The exhaust losses in DHMDC mode decrease by about 5%–8%, while the heat transfer losses increase by over 20%, resulting in a lower indicated thermal efficiency (ITE) in comparison with DMDC mode. The effects of the 20% water addition in methanol are sensitive to changes in engine load and MIT. Higher engine load and appropriately retarded MIT facilitate more efficient and cleaner combustion in DHMDC mode.

Features and Advantages of the Recurrent Approximation of Retention Times in Reversed-Phase High-Performance Liquid Chromatography

Background: Recurrent approximation of retention parameters in reversed-phase HPLC is effective for revealing anomalies that are otherwise difficult to detect, namely, the reversible hydration of analytes. This was demonstrated previously for restricted sets of analytes with acetonitrile–water eluents. Expanding the number of analytes and eluents seems to be a topical problem. Two kinds of derivatives of aromatic carbonyl compounds were characterized: unsubstituted hydrazones and oximes. Methods: If analyte demonstrates no anomalies in dependences of retention times vs. concentration of organic modifier, the recurrent approximations of these dependences are linear. To explain the features of recurrent approximations, the numerical experiments were proposed and considered. The artificial shifting of one, two, or more points allows for the modeling the different kinds of deviations of approximations from linearity. Results: It was shown that hydrazones are the class of analytes having no anomalies of retention parameters. On the contrary, several anomalies were detected for oximes. Downward deviations of points in the plots of recurrent approximations of retention times are the signs of reversible hydration. This effect for methanol–water eluents was detected for the first time. Some of oximes underwent hydrolysis. Conclusions: Recurrent approximation of retention times allows detecting chemical transformations of analytes during RP HPLC analysis.

Exploring the effects of post-distillation and post-supercritical CO2 extraction on chemical profile and biological activities of two Salvia species (S. chrysophylla and S. microstegia)

In this paper the extraction of phytoconstituents from Salvia chrysophylla and S. microstegia aerial parts was performed using maceration, supercritical carbon dioxide extraction (SCO2) and hydrodistillation. Additionally, the residual material from hydrodistillation and SCO2 was evaluated for the content in secondary metabolites. To achieve these goals Nuclear Magnetic Resonance (NMR) spectroscopy, liquid chromatography coupled with diode array and multiple stage mass spectrometry (LC-DAD-MSn) and liquid chromatography coupled with high resolution quadrupole time of flight mass spectrometry (LC-HR-QTOF) were used for the analysis of non-volatile compounds. Gas chromatography coupled with mass spectrometry (GC–MS) was adopted for the essential oil analysis. Main constituents were rosmarinic acid and luteolin-7-O-glucopyranoside, in S. microstegia while sclareol and salvigenin in S. crisophylla. Regarding essential oil composition terpine-4-ol-acetate and caryophyllene oxide were the most abundant constituents in S. microstegia and S. chrysophylla respectively. Subsequently, we determined the antioxidant capacity using different chemical assays. To establish potential other bioactivities inhibition on acetylcholinesterase (AChE), butyrylcholinesterase (BChE), tyrosinase, α-amylase and α-glucosidase, was examined. The findings revealed the water extract (WE) and methanol total extract (TE) of S. microstegia extracts, exhibited higher total phenolic contents and antioxidant activity compared to S. chrysophylla extracts. Moreover, both S. microstegia and S. chrysophylla essential oils EOs displayed significant phosphomolybdenum (PBD) activity, and their acetylcholinesterase (AChE) inhibitory activity was notably elevated and nearly equivalent, measuring 2.79 mg GALAE/g and 2.78 mg GALAE/g, respectively. These findings underscore the potential for diverse applications of these plant extracts in various industries, including pharmaceuticals and cosmeceuticals.

Charge Transfer Quenching and Maximum of a Liquid-Air Contact Line Moving over a Hydrophobic Surface.

Charge transfer when a hydrophobic fluoropolymer surface comes in contact with salt solutions of water, methanol, and glycerol is investigated. It is found that the charge transfer decreases faster with an increasing fraction of glycerol in water than it does with methanol in water. It is also demonstrated that for both mixtures, the charge transfer increases with the amount of added sodium chloride for small concentrations but then reaches a maximum and subsequently decreases. Surprisingly, this maximum charge transfer shifts toward higher salt concentrations with increasing amount of glycerol in water. However, in water-methanol mixtures, one does not observe a similar shift in charge transfer maximum toward higher salt concentrations. These observations are explained using a model, taking into account the decreased shear distance from the hydrophobic surface for which ions are removed from the electrical double layer due to an interplay of forces acting on the ions.

OVICIDAL AND LARVICIDAL EFFECTS OF A HYDROALCOHOLIC EXTRACT FROM Cyrtocarpa procera LEAVES AGAINST Haemonchus contortus

This study evaluated the ovicidal and larvicidal effects of a hydroalcoholic extract (HAE) and two fractions—one aqueous (Aq-F) and the other organic (EtOAc-F)—from dehydrated Cyrtocarpa procera leaves on Haemonchus contortus. In addition, the primary compounds in the HAE and the fractions were identified. The egg hatching inhibition (% EHI) and L3 larval mortality (% Mortality) tests were performed. The treatments used in the EHI test were HAE (12.5–200 mg mL-1), Aq-F (5 and 10 mg mL-1), and EtOAc-F (0.62–10 mg mL-1); for larval mortality, HAE (50–200 mg mL-1), Aq-F (20–40 mg mL-1), and EtOAc-F (2.5–40 mg mL-1). Thiabendazole (0.1 mg mL-1) and ivermectin (5 mg mL-1) were used as positive controls, while methanol (3 %) and distilled water were negative controls. The results were analyzed using a completely randomized design and an ANOVA. The main compounds in the extract and fractions were identified using high-performance liquid chromatography. The HAE had a 100 % ovicidal effect at the highest concentration tested, while EtOAc-F had a nearly 100 % ovicidal effect at 1.25 mg mL-1, and Aq-F displayed the lowest ovicidal effect. Regarding larval mortality, the HAE exerted a larvicidal effect close to 80 % at 100 mg mL-1, while EtOAc-F displayed a larval mortality of 71.47 % at 20 mg mL-1. The chemical analysis indicated the presence of gallic acid, derivatives of gallic acid (gallates), kaempferol rutinoside, quercetin glycoside, and luteolin glycoside. This study shows evidence of the ovicidal and larvicidal properties of C. procera, which could make it useful as a natural anthelmintic in the control of H. contortus.

Evaluation of in-vitro antibacterial activity of extracts of Calpurina aurea, Vernonia amygdalina and Rumex nepalensis in Goba district, southeastern Ethiopia

ABSTRACT The great majority of the rural populations in developing countries relies on traditional medicinal plants for treating different diseases. This study investigated the antibacterial activity of Calpurnia aurea, Vernonia amygdalina, and Rumex nepalensis collected from Goba District, Bale Zone, southeastern Ethiopia against five human bacterial test pathogens (Escherichia coli, Salmonella typhi, Staphylococcus aureus, Shigella dysenteriae and Pseudomonas aeruginosa). Plant specimens were extracted with 70% ethanol, 80% methanol, petroleum ether, and distilled water. The crude extracts were evaluated against test pathogens using agar well diffusion and micro dilution methods. The highest yield was achieved by aqueous extract of C. aurea leaf (16.6 mg/ml). The antibacterial activity of the plants’ extracts ranged from a zone of inhibition of 5.4 ± 0.4 mm to 23.0 ± 0.3 mm. Overall, the highest zone of inhibition (23 ± 0.3 mm) and the highest activity index (AI) comparable to 80% of inhibition by standard antibiotic ciprofloxacin (5 µg/disc) were revealed by the methanol extract of C. aurea leaves against S. aureus. The smallest minimum inhibitory concentration (0.78 mg/ml) was achieved by 80% methanol extracts of C. aurea roots and V. amygdalina leaves against S. aureus and E. coli, respectively. Our study revealed promising antibacterial activity of the evaluated plants.. Further studies are required to evaluate the active ingredients at the in-vitro and in-vivo levels.

Catalytic activity of modified silica gel adsorbents under conditions of methanol conversion from water-methanol waste of natural gas

The work is devoted to the analysis of factors affecting the catalytic activity of modified silica gel adsorbents under conditions of methanol conversion to dimethyl ether. The objects of the study were the initial and modified silica gel adsorbents ASM, ASM VS, BASF KC-Trockenperlen H and BASF KC-Trockenperlen WS used in the purification of methanol from water‒methanol waste of natural gas. The purpose of this paper is to study the effect of the specific surface area, elemental and phase composition, and operating time of adsorbents on the catalytic activity of modified silica gel adsorbents under conditions of methanol conversion to dimethyl ether. The composition and structural characteristics of the samples were determined by X‒ray fluorescence, X-ray diffraction analysis and low-temperature nitrogen adsorption. Based on the results of IR‒spectrometric and thermal studies, changes in the structure of the surfaces of adsorbents during their operation by various components of organic origin were evaluated. The catalytic activity of silica gel adsorbents in methanol conversion was studied in a fixed bed reactor at atmospheric pressure in the range of 120-290°C and an optimized rate of methanol-saturated nitrogen flow of 1200 ml/min. The methanol conversion process was controlled by gas‒liquid chromatography. An increase of the catalytic activity of adsorbents in methanol conversion to dimethyl ether was found in the range of ASM VS < BASF KC-Trockenperlen WS < BASF KC-Trockenperlen H < ASM. The maximum catalytic activity at 290°C was shown by the adsorbent ASM with 4.2% aluminum oxide and an amorphous structure, which significantly reduces methanol emissions into the atmosphere. For crystalline adsorbents ASM VS with an alumina content of 13.2%, the catalytic activity was minimal. It is shown that the decrease in the catalytic activity of adsorbents in gas treatment unit during operation is associated with a decrease in the value of the specific surface area of samples with a constant content of aluminum oxide and phase state, which is associated with the possible blocking of the catalytic centers of adsorbents due to the accumulation of components of organic origin in the process of natural gas purification. The establishment of factors affecting the methanol conversion to dimethyl ether on modified silica gel adsorbents will allow managing environmental risks, as well as reducing risks to humans during transportation and disposal of water-methanol waste from natural gas purification.

Development and Validation of HPLC-FLD Analysis of Perampanel in MEPS-Processed Rat Plasma Sample

Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated for bioanalytical purposes. Rats’ plasma (50 µL) was processed by microextraction packed sorbent (MEPS). The analytes were separated using a Hypersil Gold octadecyl silane column (250 × 4.6 mm internal diameter, 5 μm particle size) with isocratic elution. A mobile phase consisting of acetonitrile–methanol–water (275:275:450, v/v/v; containing 50 µL triethylamine and pH adjusted to 3.25 with orthophosphoric acid) was used in this analysis. The flow rate was 1.25 mL/min. Analytes were monitored at an excitation wavelength of 285 nm and an emission wavelength of 430 nm. The linearity range for this validated method was from 3.75 to 300 ng/mL. No endogenous peaks were found in the elution of analytes in drug-free rats’ plasma. Intra- and inter-batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria. The results indicate that the present method is simple, selective, reproducible, and suitable for the analysis of perampanel in small volume samples. The robustness of the method was accessed using MODDE® design of experiments software version 12.5.

A Multidisciplinary Approach toward CMOS Capacitive Sensor Array for Droplet Analysis.

This paper introduces an innovative method for the analysis of alcohol-water droplets on a CMOS capacitive sensor, leveraging the controlled thermal behavior of the droplets. Using this sensing method, the capacitive sensor measures the total time of evaporation (ToE), which can be influenced by the droplet volume, temperature, and chemical composition. We explored this sensing method by introducing binary mixtures of water and ethanol or methanol across a range of concentrations (0-100%, with 10% increments). The experimental results indicate that while the capacitive sensor is effective in measuring both the total ToE and dielectric properties, a higher dynamic range and resolution are observed in the former. Additionally, an array of sensing electrodes successfully monitors the droplet-sensor surface interaction. However practical considerations such as the creation of parasitic capacitance due to mismatch, arise from the large sensing area in the proposed capacitive sensors and other similar devices. In this paper, we discuss this non-ideality and propose a solution. Also, this paper showcases the benefits of utilizing a CMOS capacitive sensing method for accurately measuring ToE.

Stretching of porous poly (l-lactide-co-ε-caprolactone) membranes regulates the differentiation of mesenchymal stem cells.

Background: Among a variety of biomaterials supporting cell growth for therapeutic applications, poly (l-lactide-co-ε-caprolactone) (PLCL) has been considered as one of the most attractive scaffolds for tissue engineering owing to its superior mechanical strength, biocompatibility, and processibility. Although extensive studies have been conducted on the relationship between the microstructure of polymeric materials and their mechanical properties, the use of the fine-tuned morphology and mechanical strength of PLCL membranes in stem cell differentiation has not yet been studied. Methods: PLCL membranes were crystallized in a combination of diverse solvent-nonsolvent mixtures, including methanol (MeOH), isopropanol (IPA), chloroform (CF), and distilled water (DW), with different solvent polarities. A PLCL membrane with high mechanical strength induced by limited pore formation was placed in a custom bioreactor mimicking the reproducible physiological microenvironment of the vascular system to promote the differentiation of mesenchymal stem cells (MSCs) into smooth muscle cells (SMCs). Results: We developed a simple, cost-effective method for fabricating porosity-controlled PLCL membranes based on the crystallization of copolymer chains in a combination of solvents and non-solvents. We confirmed that an increase in the ratio of the non-solvent increased the chain aggregation of PLCL by slow evaporation, leading to improved mechanical properties of the PLCL membrane. Furthermore, we demonstrated that the cyclic stretching of PLCL membranes induced MSC differentiation into SMCs within 10days of culture. Conclusion: The combination of solvent and non-solvent casting for PLCL solidification can be used to fabricate mechanically durable polymer membranes for use as mechanosensitive scaffolds for stem cell differentiation.

Optrode-Assisted Multiparametric Near-Infrared Spectroscopy for the Analysis of Liquids

We demonstrate a sensing scheme for liquid analytes that integrates multiple optical fiber sensors in a near-infrared spectrometer. With a simple optofluidic method, a broadband radiation is encoded in a time-domain interferogram and distributed to different sensing units that interrogate the sample simultaneously; the spectral readout of each unit is extracted from its output signal by a Fourier transform routine. The proposed method allows performing a multiparametric analysis of liquid samples in a compact setup where the radiation source, measurement units, and spectral readout are all integrated in a robust telecom optical fiber. An experimental validation is provided by combining a plasmonic nanostructured fiber probe and a transmission cuvette in the setup and demonstrating the simultaneous measurement of the absorption spectrum and the refractive index of water–methanol solutions.

Ultrasound-Assisted Extraction of L-Tryptophan from Chamomile Flower: Method Development and Application for Flower Parts Characterization and Varietal Difference

Chamomile has been widely used as a functional tea due to its effects on several neurohormones, some of which are related to tryptophan. An analytical ultrasound-assisted extraction (UAE) technique was successfully optimized and validated to determine tryptophan levels in chamomile flowers. A Box-Behnken design, in conjunction with response surface methodology, was conducted based on 3 factors and 3 levels: Temperature (x1; 30, 50, and 70 °C), solvent composition (x2; 0, 40, and 80% methanol in water), and ultrasonic power (x3; 20, 60, and 100%). The main (x2) and quadratic effect of solvent (x2x2); quadratic of temperature (x1x1) and ultrasonic power (x3x3); also, the interaction of solvent-ultrasonic power (x2x3) and temperature-ultrasonic power (x1x3), significantly affected (p < 0.05) the level of L-tryptophan in the extracts. Optimum extraction conditions were achieved by applying a temperature of 54 °C for 15 min using 17% methanol in water and 69% ultrasonic power. A high recovery (94.26%) was achieved with 2 extraction cycles. The coefficient of variation (CV) demonstrated that the developed method had a satisfactory level of precision (CV < 5%) for repeatability and intermediate precision. To check the applicability of the method, the parts of 2 types of chamomile flowers (German and Roman) were evaluated. This method was successfully applied to characterize chamomile flowers based on L-tryptophan levels. HIGHLIGHTS A novel ultrasound-assisted extraction method was successfully optimized and validated for extracting L-tryptophan from chamomile flowers Solvent composition was the most influential factor in extracting L-tryptophan from chamomile flowers The level of L-tryptophan in ray and disc florets part of Roman dan German chamomile was revealed for the first time GRAPHICAL ABSTRACT

Optimization of ultrasound-aided extraction of bioactive ingredients from Vitis vinifera seeds using RSM and ANFIS modeling with machine learning algorithm

Plant materials are a rich source of polyphenolic compounds with interesting health-beneficial effects. The present study aimed to determine the optimized condition for maximum extraction of polyphenols from grape seeds through RSM (response surface methodology), ANFIS (adaptive neuro-fuzzy inference system), and machine learning (ML) algorithm models. Effect of five independent variables and their ranges, particle size (X1: 0.5–1 mm), methanol concentration (X2: 60–70% in distilled water), ultrasound exposure time (X3: 18–28 min), temperature (X4: 35–45 °C), and ultrasound intensity (X5: 65–75 W cm−2) at five levels (− 2, − 1, 0, + 1, and + 2) concerning dependent variables, total phenolic content (y1; TPC), total flavonoid content (y2; TFC), 2, 2-diphenyl-1-picrylhydrazyl free radicals scavenging (y3; %DPPH*sc), 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) free radicals scavenging (y4; %ABTS*sc) and Ferric ion reducing antioxidant potential (y5; FRAP) were selected. The optimized condition was observed at X1 = 0.155 mm, X2 = 65% methanol in water, X3 = 23 min ultrasound exposure time, X4 = 40 °C, and X5 = 70 W cm−2 ultrasound intensity. Under this situation, the optimal yields of TPC, TFC, and antioxidant scavenging potential were achieved to be 670.32 mg GAE/g, 451.45 mg RE/g, 81.23% DPPH*sc, 77.39% ABTS*sc and 71.55 μg mol (Fe(II))/g FRAP. This optimal condition yielded equal experimental and expected values. A well-fitted quadratic model was recommended. Furthermore, the validated extraction parameters were optimized and compared using the ANFIS and random forest regressor-ML algorithm. Gas chromatography-mass spectroscopy (GC–MS) and liquid chromatography–mass spectroscopy (LC–MS) analyses were performed to find the existence of the bioactive compounds in the optimized extract.

Preparation of Bio-Based Polyurethane Coating from Citrullus colocynthis Seed Oil: Characterization and Corrosion Performance.

In this study, a new epoxidized oil from Citrullus colocynthis seed oil (CCSO) was obtained for a potential application in the formulation of polyurethane coatings. Initially, the fatty acid composition of CCSO was determined by gas chromatography-mass spectrometry (GC-MS). Subsequently, the epoxidation of CCSO was performed with in situ generated peracetic acid, which was formed with hydrogen peroxide (30 wt.%) and glacial acetic acid and catalyzed with sulfuric acid. The reaction was continued at a molar ratio of 1.50:1.0 of hydrogen peroxide to double bond (H2O2:DB) for 6 h at a controlled temperature of 60 °C. The resulting epoxidized oil was then used to produce a bio-based polyol by hydroxylation. The molar ratio of epoxy groups to methanol and distilled water was maintained at 1:11:2, and the reaction was carried out for 2 h at a controlled temperature of 65 °C. The major functional groups of the epoxidized oil and its polyol were validated by Fourier-transform infrared (FT-IR) and proton nuclear magnetic resonance (1H NMR) spectroscopies. A polyurethane (PU) coating was produced from the synthesized polyol and 3HDI isocyanurate, keeping the molar ratio of NCO:OH at 1:1. The resulting PU coating was then applied to glass and aluminum panels (Al 1001). After the film was cured, the properties of the PU coating were evaluated using various techniques including pencil hardness, pendulum hardness, adhesion, gloss, chemical resistance, and EIS tests. The results show that the PU coating obtained from CCSO is a promising new raw material for coating applications.

In vitro biological activities of Combretum molle R.Br. ex G. Don (Combretaceae) against mastitis-causing organisms

Bovine mastitis, caused mostly by Staphylococcus species, has gained global importance owing to the increasing prevalence of multi-drug resistant bacteria, which comprise a risk to food security and public health. In this study, the antibacterial, anti-biofilm and quorum quenching activities of six leaf extracts of Combretum molle R.Br. ex G. Don prepared using different solvents were assessed against clinical isolates of Staphylococcus aureus and two Staphylococcus ATCC strains (S. aureus ATCC 29213 and S. epidermidis ATCC 35984). The antioxidant and anti-inflammatory activity and cytotoxicity of the extracts was also evaluated. The antibacterial and anti-biofilm potential of the extracts was determined via serial microdilution and crystal violet and INT assays. Quorum quenching activity was ascertained via inhibition of violacein production in Chromobacterium violaceum ATCC 12472. The antioxidant activity was determined using in vitro chemical assays. The 15-lipoxygenase enzyme inhibition and the nitric oxide inhibition assays were utilized to ascertain the anti-inflammatory activity of the extracts. The tetrazolium-based colorimetric (MTT) reduction assay was used to determine the cytotoxicity of the extracts against Vero African green monkey kidney cells. The antibacterial activity of the extracts was moderate to good, with minimum inhibitory concentration (MIC) values of 0.02–0.63 mg/mL. The extracts had promising biofilm inhibition (≥50 %) against four of the test strains. The effects of the extracts on the metabolic activity of the test strains showed ≥ 50 % inhibition in most of the test strains at the different test times. All extracts had moderate to excellent quorum quenching activity at different concentrations with an inhibition ranging between 32.81- 96.32 %. The methanol and cold water extracts had the best antioxidant activity against the 2, 2-diphenyl-1-picrylhydrazyl (DPPH) and 2, 2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radicals with IC50 of 7.79 and 2.34 µg/mL, respectively. The hot water extract (AQH) had the best anti-inflammatory activity in terms of 15-lipoxygenase enzyme inhibition with 85.26 % inhibition, while the methanol extract had the best nitric oxide inhibition in LPS-induced RAW 264.7 macrophages with inhibition of 96.75 % at 100 µg/mL. Selectivity index values of the extracts were as high as 50. Combretum molle, therefore, offers promising potential as a source of antibiofilm and anti-quorum sensing agents with the ability to disrupt microbial virulence factors. Additionally, the extract had good antioxidant and anti-inflammatory properties, supporting further research into its use in preventing and treating bovine mastitis.

Thermoresponsive hollow polymeric shell nano/microparticles with interconnected nanoholes

AbstractPNIPAAm‐grafted thermoresponsive hollow nano‐holed polymeric‐shell (HHPS) particles were fabricated from surface‐modified colloidal silica (CS) with poly(ethylene glycol) methyl ether‐3‐(triethoxysilyl)propyl isocyanate (PEGME‐IPTES) and 3‐(trimethoxysilyl) propyl methacrylate (MPS) as templates. The polymeric shells were then synthesized through a “grafting‐through” approach via surface‐initiated polymerization of N‐isopropyl acrylamide (PNIPAAm) using potassium persulfate (KPS) as an initiator, followed by the etching of CS with hydrofluoric acid to remove the CS core templates. CS nanoparticles and PEGME‐IPTES were presynthesized using tetraethoxysilane (TEOS) and distilled water in methanol with ammonia solution as a catalyst by the sol–gel method and using 3‐(triethoxysilyl) propyl isocyanate (IPTES) with poly(ethylene glycol) methyl ether (PEGME) in the presence of dibutyltin dilaurate. The chemical structures of bare and modified CS, PNIPAAm, PNIPAAm‐CS, and HHPS particles were characterized by FT‐IR and NMR spectroscopies. SEM and TEM images confirmed that the resulting HHPS particles had a significant number of interconnected nanoholes. To evaluate the LCST behaviors of HHPS particles, the transition of transmittance and the changes in particle diameter according to the temperature change were measured through UV‐vis spectroscopy, DLS, and microscopy.

Water detection in organic solvents using a copolymer membrane immobilised with a fluorescent intramolecular charge transfer-type dye: effects of intramolecular hydrogen bonds.

Numerous fluorescent dye-based optical sensors have been developed to detect water in organic solvents. However, only a few such sensors can detect water in polar solvents such as methanol or dimethyl sulfoxide, and their detection range is generally narrow. Therefore, in this study, a copolymer membrane incorporated with a pyridinium betaine dye (denoted PB1), which exhibited intramolecular charge transfer (ICT) characteristics, was developed to realise simple water detection in organic solvents. The pyridinium betaine structure, comprising intramolecular hydrogen bonds between the oxygen in the maleimide moiety and the hydrogen in the pyridinium, was vital for achieving efficient fluorescence emission. The membrane was prepared by copolymerising PB1 with the N,N-dimethyl acrylamide/acrylamide monomer on a glass plate, and the fluorescence in water-mixed organic solvents was investigated (λabs = 490 nm, λfl = 630 nm). The fluorescence intensity of the dye-immobilised membrane decreased with increasing water content of the organic solvents. The detection ranges in tetrahydrofuran, ethanol, methanol, and dimethyl sulfoxide were approximately <40, <40, <40, and <60 vol% water, respectively. In contrast, membranes based on a quaternary pyridinium dye (without intramolecular hydrogen bonds) did not detect water in methanol and dimethyl sulfoxide, although it was more sensitive than PB1 in the narrow region of low water concentration in THF. Theoretical calculations corroborated the importance of the pyridinium betaine structure in detecting water in organic solvents, with the increase in polarity and the formation of intermolecular hydrogen bonds between PB1 and water found to induce molecular rotation and fluorescence quenching.

A low-volume LC/MS method for highly sensitive monitoring of phenoxymethylpenicillin, benzylpenicillin, and probenecid in human serum.

Background: The optimization of antimicrobial dosing plays a crucial role in improving the likelihood of achieving therapeutic success while reducing the risks associated with toxicity and antimicrobial resistance. Probenecid has shown significant potential in enhancing the serum exposure of phenoxymethylpenicillin, thereby allowing for lower doses of phenoxymethylpenicillin to achieve similar pharmacokinetic/pharmacodynamic (PK/PD) targets. We developed a triple quadrupole liquid chromatography mass spectrometry (TQ LC/MS) analysis of, phenoxymethylpenicillin, benzylpenicillin and probenecid using benzylpenicillin-d7 and probenecid-d14 as IS in single low-volumes of human serum, with improved limit of quantification to support therapeutic drug monitoring. Methods: Sample clean-up was performed by protein precipitation using acetonitrile. Reverse phase chromatography was performed using TQ LC/MS. The mobile phase consisted of 55% methanol in water + 0.1% formic acid, with a flow rate of 0.4 mL min-1. Antibiotic stability was assessed at different temperatures. Results: Chromatographic separation was achieved within 2 minutes, allowing simultaneous measurement of phenoxymethylpenicillin, benzylpenicillin and probenecid in a single 15 μL blood sample. Validation indicated linearity over the range 0.0015-10 mg L-1, with accuracy of 96-102% and a LLOQ of 0.01 mg L-1. All drugs demonstrated good stability under different storage conditions. Conclusion: The developed method is simple, rapid, accurate and clinically applicable for the quantification of phenoxymethylpenicillin, benzylpenicillin and probenecid in tandem.