Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography

Hydrophilic interaction liquid chromatography (HILIC) has emerged in recent years as a valuable alternative to reversed-phase liquid chromatography in the analysis of polar compounds. Research in HILIC is divided into two directions: the assessment of the retention mechanism and retention behavior, and the development of HILIC methods. In this work, four polar neutral analytes (iohexol and its related compounds A, B, and C) were analyzed on two silica and two diol columns in HILIC mode with the aim to investigate thoroughly the retention mechanisms and retention behavior of polar neutral compounds on these four columns. The adsorption and partition contribution to the overall HILIC retention mechanism was investigated by fitting the retention data to linear (adsorption and partition) and nonlinear (mixed-retention and quadratic) theoretical models. On the other hand, the establishment of empirical second-order polynomial retention models on the basis of D-optimal design made possible the estimation of the simultaneous influence of several mobile-phase-related factors. Furthermore, these models were also used as the basis for the application of indirect modeling of the selectivity factor and a grid point search approach in order to achieve the optimal separation of analytes. After the optimization goals had been set, the grids were searched and the optimal conditions were identified. Finally, the optimized method was subjected to validation.

QSAR of caffeines by similarity cluster prediction

A novel QSAR approach based on correlation weighting and alignment over a hypermolecule that mimics the investigated correlational space was performed on a set of 40 caffeines downloaded from the PubChem database. The best models describing log P and LD50 values of this set of caffeine derivatives were validated against the external test set and in a new predictive model by using clusters of similarity.      

Activated carbon from bamboo waste modified with iron and its application in the study of the adsorption of arsenite and arsenate

Activated carbon obtained from bamboo waste was synthesised and modified with iron (BAC-Fe) and used for the removal of arsenic from aqueous solutions. Two different adsorption models were used for analysing the data. The adsorption capacities were determined for BAC-arsenite, BAC-Fe-arsenite, BAC-arsenate and BAC-Fe-arsenate, with a qmax (μg g^?1) of 14.89, 19.19, 22.32 and 27.32 respectively. Adsorption capacity varied as a function of pH and modifications to the sorbent. Adsorption isotherms from an aqueous solution of arsenite and arsenates on activated carbons were determined. These adsorption isotherms were consistent with the Langmuir and Freundlich adsorption models. Adsorption kinetics followed a pseudo-first order rate equation, as did the kinetics for BAC-Fe-arsenite and BAC-Fe-arsenate adsorption.      

The first synthesis of 3-deoxyoripavine and its utilization in the preparation of 10-deoxyaporphines and cyprodime

The synthesis of 3-deoxyoripavine (7) was realized as a novel and promising intermediate towards the synthesis of the important class of dopaminergic and/or serotonergic 10-deoxyaporphines and the special pharmacological tool µ opioid antagonist cyprodime. Generally, the preparation of these valuable biologically active compounds was achieved in remarkable yields.      

Equilibrium, kinetic, and thermodynamic studies of Basic Blue 9 dye sorption on agro-industrial lignocellulosic materials

The sorptive potential of some lignocellulosic agro-industrial wastes (sunflower seed shells and corn cob) for Basic Blue 9 cationic dye removal from aqueous solutions was examined using the batch technique. The Freundlich, Langmuir, and Dubinin-Radushkevich isotherm models were used in order to determine the quantitative parameters of sorption. The Langmuir isotherm model indicated a maximum sorption capacity for these materials in the range of 40–50 mg dye per g (25°C), slightly higher for corn cob than for sunflower seed shells. The values of the thermodynamic parameters showed that the retention of cationic dye is a spontaneous and endothermic process. The application of pseudo-first order and pseudo-second order intraparticle diffusion models, and a Boyd — Reichenberg model for kinetic data interpretation suggested that sorption of Basic Blue 9 dye onto the studied materials is a process where both surface sorption and intraparticle diffusion contributed to the rate-limiting step. These lignocellulosic wastes can be used with good efficiency for dye removal from aqueous effluents.      

Hydroconversion of parafine LTP56-H over nickel/Na-mordenite catalysts

Nickel catalysts supported on Na-mordenite were used for paraffin LTP56-H hydroconversion into liquid material as a possible component for engine fuels. The effects of none-catalytic thermal treatment and catalytic conditions-zeolite type and reaction conditions (solvent) on the process of liquefaction of LTP56-H paraffin and physicochemical properties of catalysts were studied. The physicochemical properties of catalytic systems were investigated using XRD, TPR, TPD-NH3 and SEM-EDS methods.      

High-pressure phase equilibrium calculations for carbon dioxide + cyclopentane binary system

The phase behavior of the carbon dioxide + cycloalkane mixtures usually receives low attention, though these systems are important for many industries, e.g. the carbon capture and storage. In this paper calculations results for the carbon dioxide + cyclopentane binary system are presented, based on SRK and PR cubic equations of state with classical van der Waals mixing rules. A single set of binary parameters for each model was proposed to predict the global phase behavior of the system in a wide range of pressure and temperature. Albeit the thermodynamic models used are simple, they are able to represent fairly well the phase behavior of the system analyzed in this paper.

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Synthesis,structure and capacitive properties of cobalt hydroxide films on stainless steel substrates

Cobalt (hydro)oxide films on AISI 304 stainless steel and sintered metal fibre filter Bekipor ST 20AL3 were prepared using electrochemical deposition from neutral cobalt acetate solutions under galvanostatic conditions. Deposited films were structurally characterized using X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. All electrochemical measurements were performed in aqueous NaOH solution. Capacitive behavior of different films was evaluated using cyclic voltammetry data. The highest specific capacitance (965 F g^?1) was reached when Bekipor ST 20AL3 mesh was used as a support for electroactive substance.      

Preparation of selectively protected protoescigenin derivatives for synthesis of escin analogs and neoglycoconjugates

Protoescigenin, the main aglycone of horse chestnut saponin mixture known as escin, was selected as substrate for exploratory chemistry towards selective protection, followed by propargyl ether formation and subsequent condensation with azido-monosaccharides, to obtain novel triazole linked conjugates of the triterpene.      

Reaction of barbituric acid with organic azides and phosphonium ylides

Amination by organic azides has been carried out to provide aminobarbiturates by fusion of a triazole ring to the 5,6-positions of barbituric acid followed by cleavage and thermal elimination of nitrogen, whereas aza-Wittig reaction gave phosphoranylidene barbituric acid salts.      

Polymer conjugates with potential biological activity based on new derivatives of 2-mercaptobenzoxazole-synthesis and characterization

New potentially biologically active compounds derived from 2-mercapto-benzoxazole were synthesized and coupled on polymeric support of poly (maleic anhydride-alt-vinyl acetate) for the preparation of polymer-drug conjugates with controlled drug release. All compounds were characterized by elemental and spectroscopy (FT-IR, ¹H-NMR) analysis. The toxicological tests recommend the products for further laboratory screening.      

Enantioselective Michael additions of aldehydes to nitroalkenes catalyzed with ionically tagged organocatalyst

Enantioselective organocatalytic Michael additions affords useful building blocks for many biologically and medicinally relevant compounds. Ionically-tagged diphenylprolinol silyl ether efficiently catalyzes several Michael additions of aldehydes to nitroalkenes in ionic liquids. The Michael additions work well in ionic liquids; yields up to 95% and enantioselectivities up to 95% ee were achieved. Furthermore, in some cases, the catalytic system was reusable.      

Application of UV detection in HPLC in the total antioxidant potential assay

HPLC has been already used for the TAP estimation. Phenylalanine, salicylic, p-hydroxybenzoic (pHBA) or terephthalic (TPA) acids have been used as sensor compounds. Products of their reaction with the hydroxyl radicals, generated in the Fenton-like reaction, were analyzed using electrochemical or fluorescence detection. This paper describes the TAP assay based on the hydroxyl radicals reaction with pHBA, reversed-phase-HPLC separation and UV photometric detection. The elaborated assay has been used to evaluate TAP values of some apiculture products.      

Salutaridine and its derivatives as thebaine-equivalents in the synthesis of aporphines

Here we report the transformation of tetracyclic morphinan salutaridine (1) into 2,3,10,11-tetrasubstituted (R)-aporphines. This method serves as another chemical proof of the previously verified biosynthetic connection with pentacyclic morphinan-6,8-diene-type thebaine. In the presence of nucleophiles, this procedure could lead to pharmacologically interesting new tetrasubstituted aporphinoids. The enantioselective synthesis of 7S-salutaridinol (2) has been also achieved in order to investigate the acid-catalyzed reactions of this natural morphinan.      

Enantioselective inhibition of immobilized acetylcholinesterase in biosensor determination of pesticides

Chiral effects for the inhibition of acetylcholinesterase by organophosphorus pesticides were investigated for insecticide malathion and malaoxon, which is a metabolic product of malathion in living organisms. Studies were carried out using a bienzymatic biosensor with immobilized acetylcholinesterase, choline oxidase, and with Prussian Blue used as a mediator. In both cases the R enantiomers accelerate acetylocholinesterase inhibition. The chiral effect in inhibition was much more pronounced in fast flow measurements than in batch measurements.      

Effect of oxidation of nitride coatings on corrosion properties of Ti-6Al-4V alloy in 0.9% NaCl at 40°C

The corrosion properties of Ti-6Al-4V alloy with oxidized thermodiffusion nitride coatings were investigated in isotonic 0.9% solution of NaCl at temperature of 40°C. It was shown that modification of nitride coatings by oxygen leads to a deterioration of the protective properties of nitrided surface of Ti-6Al-4V alloy. The protective properties of the alloy with nitride coatings modified by oxygen are determined by the composition of formed surface oxynitride film.      

In vitro biological activity comparison of some hydroxyapatite-based composite materials using simulated body fluid

Hydroxyapatite composites are the main biomaterials used for metal implant coatings. Their in vitro study is very important. That is why their behavior was monitored in simulated body fluid (SBF), which is a solution with ion concentrations and pH value similar to those of human blood plasma. Silica, chitosan and gelatin-doped hydroxyapatite-based biomaterials were studied in SBF; the samples were characterized pre-, during and post-SBF immersion using infra-red, scanning and transmission electron spectroscopy and X-ray diffraction methods. The solubility of materials in SBF was determined, and the variation of Ca²⁺ and phosphorus concentration was also recorded during SBF experiments. The results were compared and their in vitro biological activity was determined.      

Facile ultrasensitive monitoring of mercury ions in water by fluorescent ratiometric detection

Prospects for analytical application of 2,5-diphenyloxazole-substituted 3-hydroxychromone for detection of mercury ions are presented. Sensitivity and selectivity for a number of metal ions both in methanol solution and in the plasticized polymer are outlined. Ultrasensitive and highly selective fluorescent ratiometric response of the polymer film containing the title compound for mercury ions in water media is revealed. Reversibility of ratiometric response to mercury ions and influence of plasticizer’s content in the polymer film on the optical feedback are also discussed.