Ambazone salt with p-aminobenzoic acid

In this study, we obtained a novel salt of ambazone (AMB) with p-aminobenzoic acid (PABA) that exhibits improved solubility and antibacterial activity. The salt was produced by solvent-drop grinding and characterized by powder X-ray diffraction, thermal analysis and Fourier transform infrared spectroscopy. The salt nature of the new form was confirmed by infrared spectroscopy based on the characteristic vibrational band of the protonated amino group. Based on the X-ray powder diffraction data, the compound crystallizes in the triclinic P_-1 space group with the following unit cell parameters: a = 14.294 Å, b = 9.162 Å, c = 8.777 Å, α = 95.90°, β = 100.63°, γ = 91.73°. Thermal analysis reveals the thermal events and different decomposition steps of this solid form as compared to the starting compounds. Powder dissolution measurements showed solubility improvement compared with pure ambazone of 2 and 3.3 times in water and phosphate buffer, respectively. Antibacterial tests showed higher activity of the salt to Gram-negative Escherichia coli and Salmonella bacteria as compared to AMB and PABA. The study demonstrates that the pharmaceutical salt of ambazone with p-aminobenzoic acid (AMB–PABA) can be a possible alternative to ambazone in the treatment of infections with Gram-negative bacteria.     

Dioxygen Binding in the Active Site of Histone Demethylase JMJD2A and the Role of the Protein Environment

JMJD2A catalyses the demethylation of di‐ and trimethylated lysine residues in histone tails and is a target for the development of new anticancer medicines. Mechanistic details of demethylation are yet to be elucidated and are important for the understanding of epigenetic processes. We have evaluated the initial step of histone demethylation by JMJD2A and demonstrate the dramatic effect of the protein environment upon oxygen binding using quantum mechanics/molecular mechanics (QM/MM) calculations. The changes in electronic structure have been studied for possible spin states and different conformations of O₂, using a combination of quantum and classical simulations. O₂ binding to this histone demethylase is computed to occur preferentially as an end‐on superoxo radical bound to a high‐spin ferric centre, yielding an overall quintet ground state. The favourability of binding is strongly influenced by the surrounding protein: we have quantified this effect using an energy decomposition scheme into electrostatic and dispersion contributions. His182 and the methylated lysine assist while Glu184 and the oxoglutarate cofactor are deleterious for O₂ binding. Charge separation in the superoxo‐intermediate benefits from the electrostatic stabilization provided by the surrounding residues, stabilizing the binding process significantly. This work demonstrates the importance of the extended protein environment in oxygen binding, and the role of energy decomposition in understanding the physical origin of binding/recognition.     

Determination of four acidic nonsteroidal anti‐inflammatory drugs in wastewater samples by dispersive liquid–liquid microextraction based on solidification of floating organic droplet and high‐performance liquid chromatography

A simple, environmentally friendly, and sensitive dispersive liquid–liquid microextraction based on solidification of floating organic droplet for the extraction of four acidic nonsteroidal anti‐inflammatory drugs (ketoprofen, naproxen, ibuprofen, and diclofenac) from wastewater samples subsequent by high‐performance liquid chromatography analysis was developed. The influence of extraction parameters such as pH, the effect of solution ionic strength, type of extraction solvent, disperser solvent, and extraction solvent volume were studied. High enrichment factors (283–302) were obtained through the developed method. The method provides good linearity (r > 0.999) in a concentration range of 1–100 μg/L, good intra‐ and inter‐day precision (relative standard deviation < 7%) and low limits of quantification. The relative recoveries of the selected compounds were situated over 80% both in synthetic and real water samples. The developed method has been successfully applied for the analysis of the selected compounds in wastewater samples.     

WATER UPTAKE INTO STRATUM CORNEUM; PARTITION BETWEEN LIPIDS AND PROTEINS

Water uptake in natural and reaggregated stratum corneum was determined by weight difference after storage in an atmosphere of controlled relative humidity.

Interlayer spacing in separated lipids as a function of their water content was determined by low-angle X-ray diffractometry. These values were used as a calibration curve to determine the water content of the lipid bilayers in reaggregated stratum corneum.

The results revealed different behavior of the lipid models compared to natural lipids of the stratum corneum. The additional water taken up after reaggregation of equilibrated lipids and proteins, was equally partitioned between the protein and the natural lipid fraction, while the models gave a proportionally higher water uptake into the lipids at high relative humidity. It is obvious that the models, so far, do not mimic all the properties of the natural stratum corneum lipids.     

Synthesis of doubly labeled polyacrylic acid with14C and3H

Polyacrylic hydrogels were¹⁴C- and³H-labeled in three main steps. In the first one, the monomer as sodium salt was¹⁴C-labeled at the carboxyl group via the carbonation of vinylmagnesium bromide and [1-¹⁴C]acrylic acid was obtained, followed by labeling with tritium via isotopic exchange in heterogeneous catalysis. The monomer was purified and its radiochemical purity was analyzed using TLC. In the last step, the hydrogel was obtained through radiopolymerization of the doubly labeled monomer using a⁶⁰Co source. The oligomers and unpolymerized monomers were eliminated from the hydrogel by swelling in water followed by dehydration with methanol.     

Fluctuations of the second order observables for dissipative processes in 19F+27Al system

The excitation function (EF) data for dissipative processes in ¹⁹F + ²⁷Al system in the incident energy interval from 113.5 to 130 MeV are used to obtain the dependence of the charge variance and of the interaction time as a function of the incident energy. Fluctuations are observed in the EFs of both these secondary observables. Their correlation is supported by a mechanism based on stochastic exchange of nucleons.     

Nachweis und Bestimmung des Chroms

Ohne Zusammenfassung     

Thermodiffusive characteristics of some adhesive,film-forming materials and the component solvents

The TG curves obtained for various temperatures and evaporation times allowed establishment of the thermodiffusive characterics of the solvents frequently used in adhesive and film-forming materials. Determinations were carried out in air with a flow rate of 51/h, on pure solvents, on mixtures with solvent ratios corresponding to those in the final products, and on the final products. The temperature range of the study was 17–35°, the evaporation period for most cases at each temperature being 25 minutes. The method leads to the evaporation rates of such solvents with an average standard deviation of 4 per cent.