Structure and surface properties of praseodymium modified alumina

Mixed PrO₂-Al₂O₃ oxides with different PrO₂ content (1-20 wt.%) were prepared by wetness impregnation of γ-alumina with aqueous solution of praseodymium nitrate. The samples were characterized by different techniques, using surface adsorption-desorption of N₂ (S_BET), thermogravimetric analysis (TGA), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS), temperature-programmed reduction (TPR) and temperature-programmed desorption of CO₂ (TPD-CO₂). TGA and XRD showed the presence of small praseodymium oxide species on the alumina surface. XPS and DRS detected electron deficient interaction between deposited praseodymium oxide and alumina. It was observed a lower reduction temperature for supported Pr oxide species compared to that of the bulk Pr₆O₁₁. TPD-CO₂ studies suggested that the deposition of Pr oxide on alumina leaded to increase of the basicity of mixed oxides.     

New hydrofluoropolyethers II: Physico-chemical characterization

We obtained, through an original multi step synthetic approach with 60-80% selectivity, a novel family of hydrofluoropolyethers (HFPEs) characterized by a macromeric perfluoropolyether (PFPE) body end-capped, on one or both sides, by a 1,1-difluoroethoxy group. We synthesized these HFPEs trough an apparently conventional hydrogenation of PFPE precursors end-capped by reducible acyl halide groups and subsequent Cl cleavage by hydrogen, promoted by UV light in presence of hydrogen radical donor or by a metal catalytic system in presence of H₂. The physico-chemical properties of these HFPEs were described and compared to those of similar perfluorinated or partially hydrogenated molecules, obtaining master curves of general validity when temperature dependent properties, like viscosity, were compared under temperature reduced condition. The contribution of the end-groups to the specific property, vanishing at a sufficient high molecular weight, was demonstrated more and more important at the lowest oligomerization degrees.     

Development and Optimization of a Procedure for the Determination of Indium-Tin Oxide Particle Size and Concentration in Cellular Media

Indium-tin oxide (ITO) is a solid mixture often comprised of approximately 90% indium oxide and 10% tin oxide by weight. ITO is employed as a transparent conductive coating for flat panel, liquid crystal, and plasma displays and is typically deposited after sintering as a thin film on a substrate through a variety of processes. Unfortunately, there have been published reports of workers who have been adversely impacted through exposure to this compound. When these reports are coupled with the industrial utility of ITO, future toxicological investigations are likely. Comprehensive characterization of ITO test materials would be an essential component of these studies. Ideally, characterization would include assessment of ITO particle size as administered during dosing because this physicochemical parameter can significantly impact solubility. The objective of this task was to develop, optimize, and apply a dynamic light scattering (DLS) sample preparation and measurement protocol for determination of particle size for a suite of sintered/non-sintered ITO samples prepared in cellular growth media at nominal 0.3 mg/mL doses. Sonication time was evaluated from 15 to 90 minutes over a 24-hour, continuous DLS measurement period. Resulting suspensions from samples subjected to 30 minute sonication times were stable with respect to hydrodynamic particle size between 10 and 24 hours after sonication. Throughout the 24-hour DLS measurement period, suspension aliquots were analyzed by inductively coupled plasma mass spectrometry to determine indium concentration. The developed protocol enabled investigators to use ITO suspensions of known hydrodynamic particle size and concentration in their in vitro cellular study.     

Analytical tools for the physicochemical profiling of drug candidates to predict absorption/distribution

The measurement of physicochemical properties at an early phase of drug discovery and development is crucial to reduce attrition rates due to poor biopharmaceutical properties. Among these properties, ionization, lipophilicity, solubility and permeability are mandatory to predict the pharmacokinetic behavior of NCEs (new chemical entities). Due to the high number of NCEs, the analytical tools used to measure these properties are automated and progressively adapted to high-throughput technologies. The present review is dedicated to experimental methods applied in the early drug discovery process for the determination of solubility, ionization constants, lipophilicity and permeability of small molecules. The principles and experimental conditions of the different methods are described, and important enhancements in terms of throughput are highlighted. Figure Scheme of the Drug Research Process.     

甲醇对1-丁基-3-甲基咪唑四氟硼酸离子液体结构与性质影响的模拟研究

采用分子动力学模拟方法研究了298.15 K、0.1 MPa下摩尔分数为0.1-0.9 的甲醇对1-丁基-3-甲基咪唑四氟硼酸盐([BMIM][BF₄])结构与性质的影响. 获得了体系的密度、径向分布函数、配位数、自扩散系数、粘度和电导率, 模拟得到的密度值与实验值符合较好. 结果显示: 体系各组分之间的径向分布函数随甲醇摩尔分数的增加呈规律性变化; 体系内阴阳离子的自扩散系数随着甲醇摩尔分数的增加不断增大; 甲醇的加入削弱了阴阳离子之间的相互作用, 体系粘度随着甲醇摩尔分数的增加逐渐减小, 电导率不断增大. 分析空间分布函数得到体系中各组分的三维空间分布情况.     

Evaluation of poly(L-lactic acid) (PLLA) rapid indicator film on deterioration degree of Refined,Bleached and Deodorised Malaysian Tenera palm olein oil (RBDPO) during long-term repetitive deep-fat frying

Palm olein oil is widely used as a medium for deep-frying purposes in the domestic and commercial sectors. However, repetitive usage beyond the recommended cycle leads to significant deterioration and spoilage of the oil. Therefore, this research investigated the effect of long-term repetitive deep-fat frying on the physicochemical properties of Refined, Bleached and Deodorised Malaysian Tenera Palm Olein oil (RBDPO) as well as the suitability of poly(L-lactic acid) (PLLA) film as a potential rapid indicator to determine the spoilage level of recycled palm olein oil. The study was carried out using three different RBDPO conditions; RBDPO without potatoes (RBDPO-1), RBDPO with potatoes (RBDPO-2), and RBDPO with Afdhal Oil (AO, an oil additive chemical) and potatoes (RBDPO-3). The deep-frying process was performed for 15 mins at 180 ± 5 °C for 15 cycles. Based on the results, the oil temperature fluctuation during the frying process was insignificant for every cycle (p > 0.05). After 15 frying cycles, all oil samples demonstrated a considerably altered and deteriorated composition, both physically and chemically. The comparison between the 1st and 15th frying cycles showed a significant difference (p < 0.05) in the decrease of moisture content and contact angle. Furthermore, the redness colour and viscosity for RBDPO-1, RBDPO-2 and RBDPO-3 increased significantly. The RBDPO-2 recorded the highest value for moisture content, contact angle, colour and viscosity after 15 frying cycles with 30.40 ± 0.2%, 26.01 ± 0.02°, 10.77 ± 0.15 Lovibond, and 133.5 ± 0.2 cP, respectively. However, the density value was insignificant (p > 0.05) between the 1st and 15th frying cycles for all types of oil. Besides, the peroxides value (PV) was steadily increased within the safety limit of Food Act (1983) (Laws of Malaysia: Act 281), with the aldehyde (CO) functional group was detected in all oil samples throughout the 15 frying cycles. Hence, the high correlation between the contact angle and all parameters except density showed that contact angle analysis using PLLA film was a suitable technique for rapid oil spoilage indicator model.     

Fast log P determination by ultra-high-pressure liquid chromatography coupled with UV and mass spectrometry detections

Ultra-high-pressure liquid chromatography (UHPLC) systems able to work with columns packed with sub-2 μm particles offer very fast methods to determine the lipophilicity of new chemical entities. The careful development of the most suitable experimental conditions presented here will help medicinal chemists for high-throughput screening (HTS) log P _oct measurements. The approach was optimized using a well-balanced set of 38 model compounds and a series of 28 basic compounds such as β-blockers, local anesthetics, piperazines, clonidine, and derivatives. Different organic modifiers and hybrid stationary phases packed with 1.7-μm particles were evaluated in isocratic as well as gradient modes, and the advantages and limitations of tested conditions pointed out. The UHPLC approach offered a significant enhancement over the classical HPLC methods, by a factor 50 in the lipophilicity determination throughput. The hyphenation of UHPLC with MS detection allowed a further increase in the throughput. Data and results reported herein prove that the UHPLC-MS method can represent a progress in the HTS-measurement of lipophilicity due to its speed (at least a factor of 500 with respect to HPLC approaches) and to an extended field of application. Figure The UHPLC approach described here greatly enhanced the time required for log P determination (5' min by compound using UV detection) and, at least, 8 compounds measured in a 5' run when Mass Spectrometry detection in used. These developments offer to medicinal chemists a high-throughput method to estimate the lipophilicity of NCEs Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users. Experimental section for capillary electrophoresis (CE) measurements, list of the 38 compounds of the calibration set and solvatochromic analyses of the extrapolated retention factors and partition coefficients.     

Different Dimensionalities,Morphological Advancements and Engineering of g-C3N4-Based Nanomaterials for Energy Conversion and Storage

Graphitic carbon nitride (g-C₃N₄) has gained tremendous interest in the sector of power transformation and retention, because of its distinctive stacked composition, adjustable electronic structure, metal-free feature, superior thermodynamic durability, and simple availability. Furthermore, the restricted illumination and extensive recombination of photoexcitation electrons have inhibited the photocatalytic performance of pure g-C₃N₄. The dimensions of g-C₃N₄ may impact the field of electronics confinement; as a consequence, g-C₃N₄ with varying dimensions shows unique features, making it appropriate for a number of fascinating uses. Even if there are several evaluations emphasizing on the fabrication methods and deployments of g-C₃N₄, there is certainly an insufficiency of a full overview, that exhaustively depicts the synthesis and composition of diverse aspects of g-C₃N₄. Consequently, from the standpoint of numerical simulations and experimentation, several legitimate methodologies were employed to deliberately develop the photocatalyst and improve the optimal result, including elements loading, defects designing, morphological adjustment, and semiconductors interfacing. Herein, this evaluation initially discusses different dimensions, the physicochemical features, modifications and interfaces design development of g-C₃N₄. Emphasis is given to the practical design and development of g-C₃N₄ for the various power transformation and inventory applications, such as photocatalytic H₂ evolution, photoreduction of CO₂ source, electrocatalytic H₂ evolution, O₂ evolution, O₂ reduction, alkali-metal battery cells, lithium-ion batteries, lithium–sulfur batteries, and metal-air batteries. Ultimately, the current challenges and potential of g-C₃N₄ for fuel transformation and retention activities are explored.     

Acetonitrile - 2-Methyl-Propan-1-ol and Acetonitrile - 2-Methyl-Propan-2-ol Binary Mixtures and their Physicochemical Properties

The 1 H-NMR spectra of liquid binary mixtures of acetonitrile with 2-methyl-propan-1-ol (i-BtOH) and 2-methyl-propan-2-ol (t-BtOH), were recorded at 298 K over almost the whole range of mixed solvent compositions. From these data the values of spectral parameters, j i (ACN-i-BtOH) and j i (ACN-t-BtOH) were found. The relative permittivities ( k 12 ) and the densities ( d 12 ) of the mixed solvents were measured at 288.15 K, 293.15 K, 298.15 K, 303.15 K and 308.15 K. The experimental data were used to test some empirical equations of the type: y 12 = y 12 ( t ) and y 12 = y 12 ( X 1 ) [where: y 12 = d 12 or k 12 ]. From all these data, the deviations from ideality molar volumes , temperature coefficients of relative permittivities ( f 12 ) and the excess extrathermodynamic parameters were calculated. The values of these structural parameters are discussed in terms of interactions of acetonitrile with both alcohols.     

Physicochemical features and antioxidant activity of polysaccharides from Herba Patriniae by gradient ethanol precipitation

Four polysaccharides BJP50, BJP60, BJP70 and BJP80 (total named BJPs) were separated from Herba Patriniae via gradient ethanol precipitation with 50%, 60%, 70% and 80%, respectively. After decolorization and deproteinization, their physicochemical features and antioxidant activities were investigated. The results showed that the total sugar content of BJPs accounted above 50% but no protein contained, while BJP50 and BJP60 contained a small amount of uronic acid. GC analysis indicated that BJPs were mainly composed of galactose, arabinose, glucose, mannose, xylose and rhamnose. From BJP50 to BJP80, the types of monosaccharides and the content of arabinose, glucose and mannose increased but that of galactose and rhamnose decreased, and their molecular weights gradually reduced from 2.3 × 10⁶ to 4.5 × 10³. BJPs had a good thermal stability with the order of BJP80 > BJP70 > BJP60 > BJP50. The vitro bioactivity assay showed that BJP80 and BJP70 exhibited stronger scavenging capacities for DPPH, ABTS and hydroxyl free radicals than that of BJP60 and BJP50. As the concentration reached 4 mg/mL, the scavenging capacities of BJP80 and BJP70 on DPPH and hydroxyl free radical were up to 92% and 95%, respectively, and their antioxidant activities gradually approached to the positive control.