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Amidst rising natural aggregate consumption, recycling dumped waste for structural concrete effectively addresses resource scarcity and environmental contamination. Nevertheless, the adoption of toughened glass waste aggregate (TGWA) in construction remains relatively limited. This study explores the potential use of toughened glass waste (TGW) as a substitute for natural coarse aggregate (NCA) in high-performance concrete (HPC). This paper assesses the bond strength of deformed bars embedded in toughened glass waste high-performance concrete (TGW-HPC), considering different steel reinforcement diameters (8 mm and 12 mm) and various levels of TGW replacement (ranging from 0 % to 100 %). Various durability properties, including water absorption, water permeability, chloride ion penetration, and acid attack were examined. The study also investigated the microstructural characteristics of acid attacked specimens using techniques such as XRD, FTIR, and FESEM. Several important parameters, such as chloride diffusivity (D), hydraulic diffusivity (D (θ)), and permeability coefficients (K), were derived from the experimental data. The study found TGW50-HPC resulted in the highest bond strength, about 13.1 % more than the control mix. However, TGW100-HPC bond strength decreased by 17.51 % compared to the control mix. Notably, TGW100-HPC exhibited superior durability properties and showed the lowest coefficient of permeability, indicating reduced chloride ion, and water molecule transport through the interconnected pore structure. At 90 days, the TGW100-HPC mixture exhibited a strength reduction of 42.29 %, which closely resembled the 41.20 % reduction observed at 56 days. The formation of thenardite and basanite mitigate damage to the interfacial transition zone (ITZ) led to fewer micro-cracks and reduced acid ingress through the matrix. Incorporating TGWA in engineering projects can lead to cost savings through reduced raw material expenses and disposal fees, resulting in significant economic benefits and social well-being.
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Protozoal diarrhea caused by Tritrichomonas foetus (blagburni) is a prevalent, lifelong, and globally distributed burden in domestic cats. Treatment is limited to the use of 5-nitroimidazoles and treatment failure is common. The repurposed gold salt compound auranofin has killing activity against diverse protozoa in vitro but evidence of efficacy in naturally occurring protozoal infections is lacking. This exploratory study investigated the efficacy and safety of auranofin for treatment of cats with naturally occurring, 5-nitroimidazole-resistant, T. foetus infection. The minimum lethal concentration (MLC) of auranofin against 5 isolates of feline T. foetus was determined under aerobic conditions in vitro. Healthy cats and cats with T. foetus infection were treated with immediate release auranofin (range, 0.5-3â¯mg/cat for 7 days) or guar gum-coated auranofin capsules (0.5 or 3â¯mg/cat for 7 days). Adverse effects were monitored by clinical signs and clinicopathologic testing. Efficacy was determined by fecal consistency score, bowel movement frequency, and single-tube nested PCR of feces for T. foetus rDNA. Fecal samples were assayed for concentrations of auranofin, known and predicted metabolites of auranofin, gold containing molecules, and total gold content using HPLC, LC-MS, ion mobility-MS, and ICP-MS, respectively. Auranofin was effective at killing isolates of feline T. foetus at MLC ≥ 1 µg/ml. Treatment of cats with T. foetus infection with either immediate release auranofin or a colon-targeted guar gum-coated tablet of auranofin did not eradicate infection. Treatment failure occurred despite fecal concentrations of gold that met or exceeded the equivalent MLC of auranofin. Neither auranofin, known or predicted metabolites of auranofin, nor any gold-containing molecules >100â¯Da could be detected in fecal samples of treated cats. Adverse effects associated with auranofin treatment were common but minor. These studies identify that in vitro susceptibility test results of auranofin may not translate to treatment effectiveness in vivo even when achieving gold concentrations equivalent to the MLC of auranofin in the target environment. These studies further establish the absence of any predicted or unpredicted gold containing metabolites in feces after oral administration of auranofin.
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Snow (cryotolerant) algae often form red (pink) spots in mountain ecosystems on snowfields around the world, but little is known about their physiology and chemical composition. Content and composition of pigments in the cells of the cryotolerant green microalgae Chloromonas reticulata have been studied. Analysis of carotenoids content in the green (vegetative) cells grown under laboratory conditions and in the red resting cells collected from the snow surface in the Subpolar Urals was carried out. Carotenoids such as neoxanthin, violaxanthin, anteraxanthin, zeaxanthin, lutein, and ß-carotene were detected. Among the carotenoids, the ketocarotenoid astaxanthin with high biological activity was also found. It was established that cultivation of the algae at low positive temperature (6°C) and moderate illumination (250 µmol quanta/(m2â s) contributed to accumulation of all identified carotenoids, including extraplastidic astaxanthin. In addition to the pigments, fatty acids accumulated in the algae cells. The data obtained allow us to consider the studied microalgae as a potentially promising species for production of carotenoids.
Sujet(s)
Caroténoïdes , Microalgues , Caroténoïdes/métabolisme , Caroténoïdes/composition chimique , Microalgues/métabolisme , Chlorophyta/métabolisme , Chlorophyta/composition chimique , Basse température , Xanthophylles/métabolismeRÉSUMÉ
Organophosphate nerve agents (OPs) are widely used as pesticides and chemical agents and pose a threat to human health and life. At present, most personal protective equipment usually only serves as physical protection and does not have an effect of chemical detoxification. In this work, ultra lightweight graphene oxide aerogels (GAs) have been used as a multifunctional skeleton to integrate the metal-organic frameworks (MOFs) and molecularly imprinted polymers (MIPs) together for obtaining a high-performance hybrid material (MOFs/MIPs@GAs) on hydrolysis detoxification of OPs. As a porous three-dimensional material full of carboxyl groups, GAs can not only support excellent mass transfer performance but also provide a proper pH self-buffering catalytic reaction external environment for hydrolyzing OPs. The obtained MOFs/MIPs@GAs can catalyze dimethyl-4-nitrophenyl phosphate (DMNP) hydrolysis detoxification rapidly in pure water (kobs = 0.2227 min-1, t1/2 = 3.11 min). This ternary hybrid material with exceptional performance and practical applicability has vast application prospects for the development of protective equipment.
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Sustainable hydrogen production is focused on anion exchange membrane (AEM) water electrolyzers (AEMWEs), which still require more development to achieve high performance and durability. Here, we propose a novel class of porous organic polymers (POPs) as durable solid-ionomers for AEMWEs, which was prepared by reacting the 4-methylpiperidone with trifunctional or a mixture of trifunctional:difunctional aromatic monomers (in a 2:3 mol ratio). The resulting POP ionomers exhibited exceptional electrochemical properties and remarkable alkaline stability. Particularly noteworthy are the corresponding AEMWEs, which showed an outstanding current density of 13.4 A cm-2 at 2.0 V under 80°C in 1 M KOH solution, which is the highest performance reported in the particulate-ionomers AEMWE state of the art. Moreover, they demonstrated durability at a current density of 0.5 A cm-2 for over 500 hours with a voltage decay rate of 120 µV h-1. This work offers valuable perspectives on the designing of robust and high-performance solid-state ionomers through low-cost electrophilic aromatic substitution reactions for high-performance energy conversion devices.
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In the rapidly evolving field of bioimaging, the integration and orchestration of findable, accessible, interoperable, and reusable (FAIR) image analysis workflows remains a challenge. We introduce BIOMERO (bioimage analysis in OMERO), a bridge connecting OMERO, a renowned bioimaging data management platform; FAIR workflows; and high-performance computing (HPC) environments. BIOMERO facilitates seamless execution of FAIR workflows, particularly for large datasets from high-content or high-throughput screening. BIOMERO empowers researchers by eliminating the need for specialized knowledge, enabling scalable image processing directly from OMERO. BIOMERO notably supports the sharing and utilization of FAIR workflows between OMERO, Cytomine/BIAFLOWS, and other bioimaging communities. BIOMERO will promote the widespread adoption of FAIR workflows, emphasizing reusability, across the realm of bioimaging research. Its user-friendly interface will empower users, including those without technical expertise, to seamlessly apply these workflows to their datasets, democratizing the utilization of AI by the broader research community.
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Given the limited specificity and accuracy observed in the current official colorimetric quantification of polysaccharide in Lycium barbarum, our study aims to establish a novel, specific, accurate, and economic pre-column derivatization ultra-high-performance liquid chromatography (UHPLC) method for determining the monosaccharide and polysaccharide content in L. barbarum. The optimization of extraction, hydrolysis, and derivatization (using 1-phenyl-3-methyl-5-pyrazolone) processes for polysaccharide from L. barbarum was conducted initially, followed by separation of nine monosaccharides within 20 min using UHPLC with a C18 column. Subsequently, a novel method known as quantitative analysis of multiple components by single marker was developed, utilizing either additive 2-deoxy-D-ribose or any monosaccharide present in the sample as a single reference standard to simultaneously detect the contents of polysaccharide and nine monosaccharides in L. barbarum. To validate the accuracy of the established method, the quantitative results of our approach were compared to both external and internal standard method methods. The minimal relative errors in the quantitative determination of monosaccharides among the three methods confirmed the dependability of the method. By analyzing 20 batches of L. barbarum samples, D-galacturonic acid exhibited the highest content and the polysaccharide levels ranged from 3.02 to 13.04 mg/g. All data implied the specificity and accuracy of the method.
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Lycium , Oses , Polyosides , Chromatographie en phase liquide à haute performance/méthodes , Lycium/composition chimique , Oses/analyse , Oses/composition chimique , Polyosides/analyse , Polyosides/composition chimique , Médicaments issus de plantes chinoises/composition chimique , Médicaments issus de plantes chinoises/analyseRÉSUMÉ
BACKGROUND: ß-nicotinamide mononucleotide stands out as an essential breakthrough in "anti-aging" and consistently leads the list of top-selling nutritional supplements in terms of quantity. As the metabolites of ß-nicotinamide mononucleotide, the detection of nicotinamide and N1-methylnicotinamide is of great significance for evaluating the nutritional effect of dietary supplements of ß-nicotinamide mononucleotide. However, due to the extremely low concentration of nicotinamide and N1-methylnicotinamide in vivo and the serious matrix interference in biological samples, there is an increasing demand for materials and methods of pre-treatment. RESULTS: In this study, Fe3O4@hydroxypropyl methyl cellulose@dodecylbenzenesulfonic acid magnetic fluid was synthesized for the first time, and it was used as pretreatment material to detect nicotinamide and N1- methylnicotinamide in urine samples by high performance liquid chromatography. Compared with other adsorption materials, Fe3O4@hydroxypropyl methyl cellulose@dodecylbenzenesulfonic acid nanoparticles are a kind of uniform magnetic fluid. Furthermore, they have more types and quantities of interaction sites (electrostatic interactions, hydrophobic interactions, hydrogen bonding interactions, and π-π interactions), so they own greater adsorption capacity. When the pH of the solution is 4, they can be adsorbed quickly within 10 s. The method successfully detected trace nicotinamide and N1-methylnicotinamide in urine samples in the linear range of 0.1-80 µg mL-1, the low detection limits were 0.30 ng mL-1 and 1.5 ng mL-1 respectively, and the quantification limits were 1.0 ng mL-1 and 5.0 ng mL-1, respectively. At the same time, the standard urine samples of nicotinamide and N1-methylnicotinamide showed satisfactory recovery rate 94.50-109.1 %. The results indicated that the established method can accurately and quantitatively determine trace nicotinamide and N1-methylnicotinamide in urine samples. SIGNIFICANCE: Consequently, low concentration of ß-nicotinamide mononucleotide metabolites can be detected simultaneously, and the interference can be eliminated during the detection process, which provides an efficient and convenient pretreatment method and a rapid and sensitive detection method for the analysis of ß-nicotinamide mononucleotide metabolites. What's more, it has a wide application prospect in the analysis of other similar metabolites in biological samples.
Sujet(s)
Nicotinamide , Nicotinamide mononucléotide , Nicotinamide mononucléotide/composition chimique , Nicotinamide mononucléotide/urine , Nicotinamide mononucléotide/métabolisme , Humains , Nicotinamide/urine , Nicotinamide/analogues et dérivés , Nicotinamide/métabolisme , Nicotinamide/analyse , Nicotinamide/composition chimique , Chromatographie en phase liquide à haute performance , Nanoparticules de magnétite/composition chimique , Adsorption , Limite de détectionRÉSUMÉ
Because of rapid industrialization and agriculturalization, solving the pressing problems of environment pollution, especially water and food quality, requires innovative solutions. In this paper, a novel and versatile metal-organic framework (ZIF-8)-hybrid monolithic column (ZIF-HMC) was prepared for in-tube solid-phase microextraction (IT-SPME) of organic nitrogen pesticides (ONPs). The prepared monolithic columns had superior adsorption sites, high porosity, excellent permeability, and ideal specific surface area based on Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Thermal Field Emission Scanning Electron Microscopy (SEM), Energy Dispersive Spectrometry (EDS), X-ray Photoelectron Spectroscopy (XPS), and N2 adsorption-desorption. The ZIF-HMC contained a large number of nitrogen and oxygen atoms, benzene rings and ZIF-8, which could synergistically promote the adsorption efficiency of ONPs through multiple interactions, such as hydrogen bonding, π-π accumulation, hydrophobic interactions, cation-π interactions, and pore adsorption by MOFs. Under the optimal conditions, a simple, efficient, and sensitive method for the analysis of six organic pesticides in environmental water samples was developed by using the ZIF-HMC as the extraction medium coupled with high performance liquid chromatography-ultraviolet (HPLC-UV). The method had a wide linear range (0.63-1000 µg L-1), a low detection limit (0.19-1.91 µg L-1) and satisfactory recoveries (87.4 %-110.2 %), the linear correlation coefficient was (R2) 0.9972-0.9995 and the relative standard deviation (RSD) was less than 2.64 %. The study had demonstrated the potential application of the developed method for the enrichment and analysis of organic pesticides in complex matrices of environmental samples, as well as the feasibility of MOFs materials for IT-SPME sample preparation.
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Formamidinium lead iodide (FAPbI3) perovskite has lately surfaced as the preferred contender for highly proficient and robust perovskite solar cells (PSCs), owing to its favorable bandgap and superior thermal stability. Nevertheless, volatilization and migration of iodide ions (I-) result in non-radiating recombination centers, and the presence of large formamidine (FA) cations tends to cause lattice strain, thereby reducing the power conversion efficiency (PCE) and stability of PSCs. To solve these problems, the lead formate (PbFa) is added into the perovskite solution, which effectively mitigates the halogen vacancy and provides tensile strain outside the perovskite lattice, thereby enhancing its properties. The strong coordination between the CâO of HCOO- and Pb-I backbones effectively immobilizes anions, significantly increases the energy barrier for anion vacancy formation and migration, and reduces the risk of lead ion (Pb2+) leakage, thereby improving the operation and environmental safety of the device. Consequently, the champion PCE of devices with Ag electrodes can be increased from 22.15% to 24.32%. The unencapsulated PSCs can still maintain 90% of the original PCE even be stored in an N2 atmosphere for 1440 h. Moreover, the target devices have significantly improved performance in terms of light exposure, heat, or humidity.
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Currently, deep learning is developing rapidly in the field of image segmentation, and medical image segmentation is one of the key applications in this field. Conventional CNN has achieved great success in general medical image segmentation tasks, but it has feature loss in the feature extraction part and lacks the ability to explicitly model remote dependencies, which makes it difficult to adapt to the task of human organ segmentation. Although methods containing attention mechanisms have made good progress in the field of semantic segmentation, most of the current attention mechanisms are limited to a single sample, while the number of samples of human organ images is large, ignoring the correlation between the samples is not conducive to image segmentation. In order to solve these problems, an internal and external dual-attention segmentation network (IEA-Net) is proposed in this paper, and the ICSwR (interleaved convolutional system with residual) module and the IEAM module are designed in this network. The ICSwR contains interleaved convolution and hopping connection, which are used for the initial extraction of the features in the encoder part. The IEAM module (internal and external dual-attention module) consists of the LGGW-SA (local-global Gaussian-weighted self-attention) module and the EA module, which are in a tandem structure. The LGGW-SA module focuses on learning local-global feature correlations within individual samples for efficient feature extraction. Meanwhile, the EA module is designed to capture inter-sample connections, addressing multi-sample complexities. Additionally, skip connections will be incorporated into each IEAM module within both the encoder and decoder to reduce feature loss. We tested our method on the Synapse multi-organ segmentation dataset and the ACDC cardiac segmentation dataset, and the experimental results show that the proposed method achieves better performance than other state-of-the-art methods.
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The approaches to matrix effects determination and reduction in ultra-high performance supercritical fluid chromatography with mass spectrometry detection have been evaluated in this study using different sample preparation methods and investigation of different calibration models. Five sample preparation methods, including protein precipitation, liquid-liquid extraction, supported liquid extraction, and solid phase extraction based on both "bind and elute" and "interferent removal" modes, were optimized with an emphasis on the matrix effects and recovery of 8 forms of vitamin E, including α-, ß-, γ-, and δ-tocopherols and tocotrienols, from plasma. The matrix effect evaluation included the use and comparison of external and internal calibration using three models, i.e., least square with no transformation and no weighting (1/x0), with 1/x2 weighting, and with logarithmic transformation. The calibration model with logarithmic transformation provided the lowest %-errors and the best fits. Moreover, the type of the calibration model significantly affected not only the fit of the data but also the matrix effects when evaluating them based on the comparison of calibration curve slopes. Indeed, based on the used calibration model, the matrix effects calculated from calibration slopes ranged from +92% to - 72% for α-tocopherol and from -77% to +19% in the case of δ-tocotrienol. Thus, it was crucial to calculate the matrix effect by Matuszewski's post-extraction approach at six concentration levels. Indeed, a strong concentration dependence was observed for all optimized sample preparation methods, even if the stable isotopically labelled internal standards (SIL-IS) were used for compensation. The significant differences between individual concentration levels and compounds were observed, even when the tested calibration range covered only one order of magnitude. In methods with wider calibration ranges, the inappropriate use of calibration slope comparison instead of the post-extraction addition approach could result in false negative results of matrix effects. In the selected example of vitamin E, solid-phase extraction was the least affected by matrix effects when used in interferent removal mode, but supported liquid extraction resulted in the highest recoveries. We showed that the calibration model, the use of a SIL-IS, and the analyte concentration level played a crucial role in the matrix effects. Moreover, the matrix effects can significantly differ for compounds with similar physicochemical properties and close retention times. Thus, in all bioanalytical applications, where different analytes are typically determined in one analytical run, it is necessary to carefully select the data processing in addition to the method for the sample preparation, SIL-IS, and chromatography.
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As a fruit and vegetable crop, the ornamental pepper is not just highly ornamental but also rich in nutritional value. The quality of ornamental pepper fruits is given in their contents of capsaicin, vitamin C (VC), flavonoids and total phenols. The study concentrated on the accumulation of capsaicin and dihydrocapsaicin in different tissues of 18 peppers during fruit growth and development. The results showed that the pericarp and placenta contained significantly higher levels of capsaicin than dihydrocapsaicin. Additionally, the placenta contained significantly higher levels of both capsaicin and dihydrocapsaicin compared to the pericarp. The content of capsaicin was in the range of 0-6.7915 mg·g-1, the range of dihydrocapsaicin content was 0-5.329 mg·g-1. Interestingly, we found that the pericarp is rich in VC (5.4506 mg·g-1) and the placenta is high in flavonoids (4.8203 mg·g-1) and total phenols (119.63 mg·g-1). The capsaicin is the most important component using the correlation analysis and principal component analysis. The qPCR results substantiated that the expression of genes in the placenta was significantly higher than that in the pericarp and that the expression of genes in green ripening stage was higher than that in red ripening stage. This study could be utilized to select the best ripening stages and tissues to harvest peppers according to the use of the pepper and to the needs of producers. It not only provides a reference for quality improvement and processing for consumers and market but also provides a theoretical basis for high-quality pepper breeding.
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Three-dimensional printing technology in construction is a rapidly growing field that offers innovative opportunities for design and construction execution. A key component of this process is the automated production of high-performance construction mixtures that meet specific requirements for strength, fluidity, and setting speed. This overview article outlines the history and development of 3D printing technology in the construction industry, describes various printing technologies, and discusses the properties and requirements for construction mixes. Special attention is given to automated systems for batching and mixing ingredients, which increase the precision and efficiency of production. The different types of construction mixes used in 3D printing and the main technical and operational challenges associated with their application are also presented. The article's conclusions highlight the potential of this technology to revolutionize the construction industry by improving efficiency and reducing costs and project lead times.
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A novel magnetic nanomaterial with Fe3O4 as the core, PS-DVB as the shell layer, and the surface modified with C18 (C18-PS-DVB-Fe3O4) had been synthesized by seeded emulsion polymerization. C18-PS-DVB-Fe3O4 retains the advantages of the chemical stability, large porosity, and uniform morphology of organic polymers and has the magnetic properties of Fe3O4. A simple, flexible, and efficient magnetic dispersive solid phase extraction (Mag-dSPE) method for the extraction of preservatives, sweeteners, and colorants in river water was established. C18-PS-DVB-Fe3O4 was used as an adsorbent for Mag-dSPE and was coupled with high-performance liquid chromatography (HPLC) to detect 11 food additives: acesulfame, amaranth, benzoic acid, tartrazine, saccharin sodium, sorbic acid, dehydroacetic acid, sunset yellow, allura red, brilliant blue, and erythrosine. Under the optimum extraction conditions, combined with ChromCoreTMAQC18 (5 µm, 4.6 × 250 mm), 20 mmol/L ammonium acetate aqueous solution and methanol were used as mobile phases, and the detection wavelengths were 240 nm and 410 nm. The limits of detection (LODs) of 11 food additives were 0.6-3.1 µg/L with satisfactory recoveries ranging from 86.53% to 106.32%. And the material could be reused for five cycles without much sacrifice of extraction efficiency. The proposed method has been used to determine food additives in river water samples, and results demonstrate the applicability of the proposed C18-PS-DVB-Fe3O4 Mag-dSPE coupled with the HPLC method to environment monitoring analysis.
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Background Sickle cell disease (SCD) is a significant health concern, particularly due to the variability in disease severity and frequency of crisis episodes among patients. Accurate assessment of HbS concentrations is crucial for understanding the disease's progression and severity. This study aimed to assess and evaluate HbS concentrations in sickle cell patients and those experiencing sickle cell crisis using high-performance liquid chromatography (HPLC). The objectives included screening individuals for SCD, diagnosing the disease using Hb electrophoresis, estimating HbS concentration via HPLC, and comparing HbS concentration values between sickle cell patients and those in crisis. Methods An analytical study design was employed at Jawaharlal Nehru Medical College, Sawangi, Wardha, Maharashtra, involving 80 participants diagnosed with SCD. Data collection included clinical assessments, routine sickling tests, Hb electrophoresis, and HPLC for HbS concentration measurement. Descriptive and inferential statistics were utilized for data analysis, including chi-square tests, Mann-Whitney U tests, and regression analyses. Results Significant differences in HbS concentrations were observed between different patient groups. Individuals with the SS pattern exhibited higher HbS levels than those with the AS pattern (p = 0.001). Non-crisis patients had significantly higher mean HbS concentrations than crisis patients (p = 0.001). A moderate positive correlation (0.476, p = 0.001) was found between HbS concentrations and clinical outcomes. No significant differences in HbS concentrations were noted based on sex or age group. Longitudinal analysis revealed a significant increase in HbS levels over time (p = 0.001). Conclusion The study underscores the importance of HbS concentration measurement in understanding the severity and progression of SCD. HPLC proves to be a valuable tool in accurately estimating HbS levels, aiding in better clinical management of the disease.
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A covalent organic framework (COF) was gown on porous silica with 1,3,5-tri(4-aminophenyl)benzene and 2,5-divinyl-1,4-phenyldiformaldehyde as monomers, and two ionic liquids were grafted to COF by a click reaction. The materials before and after the modification of ionic liquids were separately packed into solid-phase extraction columns (10 × 4.6 mm, i.d.), which were coupled with liquid chromatography to construct online analysis systems. The extraction mechanisms of polycyclic aromatic hydrocarbons, bisphenols, diphenylalkanes and benzoic acids were investigated on these materials. There were π-π, hydrogen-bond and electrostatic interactions on ionic liquid-functionalized sorbents. After the comparison among these materials, the best sorbent was used, and the analytical method was established and successfully applied to the detection of some estrogens from actual samples. For the analytical method, the detection limit was as low as 0.005 µg L-1, linear range was as wide as 0.017-10.0 µg L-1, and enrichment ratio was as high as 3635. The recoveries in actual samples were 70 %-129 %.
Sujet(s)
Liquides ioniques , Limite de détection , Silice , Extraction en phase solide , Liquides ioniques/composition chimique , Extraction en phase solide/méthodes , Silice/composition chimique , Hydrocarbures aromatiques polycycliques/isolement et purification , Hydrocarbures aromatiques polycycliques/analyse , Hydrocarbures aromatiques polycycliques/composition chimique , Réseaux organométalliques/composition chimique , Adsorption , Oestrogènes/isolement et purification , Oestrogènes/analyse , Oestrogènes/composition chimique , Porosité , Chromatographie en phase liquide à haute performance/méthodesRÉSUMÉ
Metal oxide materials processed using solution methods have garnered significant attention due to their ability to efficiently and affordably create transparent insulating layers or active channel layers on various substrates for thin-film transistors (TFTs) used in modern electronics. The key properties of TFTs largely depend on how charge carriers behave near the thin layer at the semiconductor and dielectric interface. Effectively controlling these characteristics offers a straightforward yet effective approach to enhancing device performance. In this study, we propose a novel strategy utilizing atmospheric pressure plasma (APP) treatment to modulate the electrical properties of dielectric thin films and the interfaces between dielectric and semiconductor layers in TFTs processed by using solution methods. Through APP exposure, significant improvements in key TFT parameters were achieved for solution-processed TFTs. Interface states have been reduced from 1013 to 1011 cm-2, and the on/off current ratio has increased from 103 to 106 while maintaining a high field-effect mobility of 34 cm2 V-1 s-1. Additionally, UV-visible spectroscopy and X-ray analysis have confirmed the effectiveness of APP treatment in controlling interface states and traps, leading to overall performance enhancements in the TFTs. Furthermore, our experimental findings have been systematically validated using technology computer-aided design (TCAD) simulations of fabricated TFTs.
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Macrocycles play vital roles in supramolecular chemistry and chromatography. 1,1'-Bi-2-naphthol (BINOL)-based chiral polyimine macrocycles are an emerging class of chiral macrocycles that can be constructed by one-step aldehyde-amine condensation of BINOL derivatives with other building blocks. These macrocycles exhibit good characteristics, such as facile preparation, rigid cyclic structures, multiple chiral centers, and defined molecular cavities, that make them good candidates as new chiral recognition materials for chromatographic enantioseparations. In this study, a BINOL-based [2+2] chiral polyimine macrocycle was synthesized by one-step condensation of enantiopure (S)-2,2'-dihydroxy-[1,1'-binaphthalene]-3,3'-dicarboxaldehyde with (1R,2R)-1,2-diaminocyclohexane. The product was modified with 5-bromo-1-pentene and then attached to thiolated silica using click chemistry to construct a new chiral stationary phase (CSP). The enantioselectivity of the new CSP was explored by separating various racemates under normal phase (NP) and reversed phase (RP) high performance liquid chromatography (HPLC). Thirteen racemates and eight racemates were enantioseparated under the two separation modes, respectively, including chiral alcohols, phenols, esters, ketones, amines, and organic acids. Among them, nine racemates achieved baseline separation under NP-HPLC and seven racemates achieved baseline separation under RP-HPLC. High resolution separation was observed with benzoin (Rs = 5.10), epinephrine (Rs = 4.98), 3-benzyloxy-1,2-propanediol (Rs = 4.42), and 4,4'-dimethylbenzoin (Rs = 4.52) in NP-HPLC, and with 4-methylbenzhydrol (Rs = 4.72), benzoin ethyl ether (Rs = 3.79), 1-phenyl-1-pentanol (Rs = 3.68), and 1-(3-bromophenyl)ethanol (Rs = 3.60) in RP-HPLC. Interestingly, the CSP complemented Chiralcel OD-H, Chiralpak AD-H, and CYCLOBOND I 2000 RSP columns for resolution of these test racemates, separating several racemic compounds that could not be well separated by the three commercially available columns. The influences of injected sample amount on separation were also evaluated. It was found that the column exhibited excellent stability and reproducibility after hundreds of injections, and the relative standard deviations (n = 5) of the retention time and resolution were less than 0.49% and 0.69%, respectively. This study indicates that the BINOL-based chiral macrocycle has great potential for HPLC enantioseparation.
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Composés macrocycliques , Naphtols , Silice , Chromatographie en phase liquide à haute performance/méthodes , Stéréoisomérie , Naphtols/composition chimique , Naphtols/isolement et purification , Composés macrocycliques/composition chimique , Composés macrocycliques/isolement et purification , Silice/composition chimiqueRÉSUMÉ
A new method for efficiently selecting polypotent natural products is proposed in this study. The method involves using effect-directed HPTLC data and multiobjective optimization algorithms to extract chromatographic signals from HPTLC bioassay images. Three different multiobjective optimization methods, namely Derringer's desirability approach, Technique for order of preference by similarity to ideal solution (TOPSIS), and Sum of ranking differences (SRD), were applied to the chromatographic signals. In combination with jackknife cross-validation, Derringer's approach and TOPSIS demonstrated high similarity in finding the best (most polypotent), next to the best, next to the worst, and worst (least polypotent) extracts, while the SRD resulted in slightly different outcomes. Furthermore, a new method for identifying the chromatographic features that characterize the most polypotent extracts was proposed. This method is based on partial least square regression (PLS) and can be used in combination with HPTLC-chemical fingerprints to predict the desirability of new extracts. The resulting PLS models demonstrated high statistical performance with determination coefficients ranging from R2 = 0.885 in the case of Derringer's desirability, to 0.986 for TOPSIS. However, the PLS modeling of SRD values was not successful.