Rheological properties of polyacrylates used as synthetic road binders

Most adhesives and binders, including bitumen for asphalt mixture production, are presently produced from petrochemicals after the refining of crude oil. The fact that crude oil reserves are a finite resource means that in the future, it may become necessary to produce these materials from alternative and probably renewable sources. Suitable resources of this kind may include polysaccharides, plant oils and proteins. This paper deals with the synthesis of polymer binders from monomers that could, in future, be derived from renewable resources. These binders consist of polyethyl acrylate (PEA) of different molecular weight, polymethyl acrylate (PMA) and polybutyl acrylate (PBA), which were synthesised from ethyl acrylate, methyl acrylate and butyl acrylate, respectively, by atom transfer radical polymerisation. The rheological properties of these binders were determined by means of oscillatory testing using a dynamic shear rheometer and combinations of stress/strain, temperature and frequency sweeps. The results indicate that PEA can be produced to have rheological properties similar to that of ‘soft’ 100/150 penetration grade bitumen, PMA with similar rheological properties to that of ‘hard’ 10/20 penetration grade bitumen, while PBA, due to its highly viscous nature and low dynamic moduli, cannot be used on its own as a binder. The synthetic polymers were found to be thermo-rheologically simple, and the shift factors, used to produce the dynamic moduli master curves, were found to fit an Arrhenius function.     

Production of carrier-free scandium radioisotopes from a neutron-irradiated potassium titanium oxalate target

Summary Extraction of scandium and calcium radioactivities with 1% HDEHP in benzene from nitric acid solution was investigated. The effect of potassium titanium oxalate concentration on the extraction from 1.5M nitric acid was studied. From the data obtained, two procedures based on batch solvent extraction and extraction chromatography were developed for separation and production of radioscandium from a neutron-irradiated potassium titanium oxalate target. The radiochemical purity of the separated scandium radioactivities was more than 98%.

---

Zusammenfassung Die Extraktion der Aktivitäten des Scandiums und Calciums aus salpetersaurer Lösung mit 1% Diäthylhexylphosphorsäure in Benzol wurde untersucht. Der Einfluß der Kalium-Titanoxalat-Konzentration auf die Extraktion aus 1,5-m Salpetersäure wurde geprüft. Auf Grund der Ergebnisse wurden zwei Verfahren zur Trennung und Gewinnung von Radio-Scandium aus einem neutronenbestrahlten Kalium-Titanoxalat-Target ausgearbeitet, die auf einmaliger Extraktion mit dem Lösungsmittel bzw. auf Extraktionschromatographie beruhen. Die radiochemische Reinheit der Sc-Aktivitäten war besser als 98%.

     

Die Veresterungsgeschwindigkeiten der Monoaminobenzoesäuren und der 1- und 2-Pyridinkarbonsäuren in Glykol und Glyzerin

Zusammenfassung Es werden die Veresterungsgeschwindigkeiten der Monoaminobenzoesäuren und der 1- und 2-Pyridinkarbonsäuren bei 25° mit Chlorwasserstoff als Katalysator sowohl in wasserfreiem als auch in wasserhaltigem Glykol und in wasserfreiem Glyzerin gemessen, die derm- und derp-Aminobenzoesäure und der 2-Pyridinkarbonsäure (Nikotinsäure) auch in wasserhaltigem Glyzerin. Die Abhängigkeit der monomolekularen Geschwindigkeitskonstanten vom Wassergehalt (w) des Mediums und dem Überschuß der Konzentration der Salzsäure über die der organischen Säure, bzw. ihres Esters (C) wird für die drei zuletzt genannten Säuren durch Formeln dargestellt. Diese Geschwindigkeitskonstanten nehmen durchwegs sowohl in wasserfreiem als auch in wasserhaltigem Glykol und Glyzerin nicht nur rascher als die Konzentration der gesamten Salzsäure, sondern auch als die des obigen Überschusses, d. h. der freien Salzsäure, zu.FürC=1/3 sind beiw=0.03 die Geschwindigkeitskonstanten derm- und derp-Aminobenzoesäure und der Nikotinsäure in Äthylalkohol um 20–30 %, die der Anthranilsäure um 70%, die der Pikolinsäure um 130% größer als in Glykol, beiw=0.7 dagegen die der drei ersteren Säuren um 35–50% kleiner.In Glykol sind die Konstanten bei der Anthranilsäure und den Pyridinkarbonsäuren kleiner als in Glyzerin, bei den übrigen wie bei den früher untersuchten Säuren aber größer.Die sterische Wirkung der Aminogruppe in Orthostellung ist in Glykol größer, in Glyzerin kleiner als in Äthylalkohol.Unter gleichen Bedingungen Bind die Konstanten der Veresterungsgeschwindigkeit der Nikotinsäure in Glykol und Glyzerin etwa viermal, in Äthylalkohol nur etwa zweimal größer als die der Pikolinsäure.     

Preparation of234Th(UX1) by extraction of238U. determination of thorium with arsenazo-III

Summary Radiochemical procedures have been worked out to prepare²³⁴Th(UX₁) with and without carrier from uranium using N-oxide of 4-(5-nonyl)pyridine in sulphuric acid media. This reagent has also been employed in the development of a combined solvent extraction-ion exchange-spectrophotometric method for the determination of thorium in various samples.

---

Zusammenfassung Radiochemische Methoden zur Herstellung von²³⁴Th(UX₁) aus Uran mit und ohne Träger und unter Verwendung von 4-(5-Nonyl)pyridin-N-oxid in schwefelsaurer Lösung wurden ausgearbeitet. Dieses Reagens wurde auch für die Ausarbeitung einer Thoriumbestimmung in verschiedenartigen Proben auf der Grundlage von Extraktion, Ionenaustausch und Spektro-photometrie verwendet.

     

Positive and negative ion mass spectra of oxygen,sulphur and selenium 2,1,3-benzodiazoles

The 70 eV positive and negative ion mass spectra of the oxygen, sulphur and selenium 2,1,3-benzodiazoles have been studied. The influence of hetero atom on the fragmentation modes of the benzodiazole molecular ions has been discussed.     

Carnosic Acid Encapsulated in Albumin Nanoparticles Induces Apoptosis in Breast and Colorectal Cancer Cells

Carnosic acid (CA) is a natural phenolic compound with several biomedical actions. This work was performed to study the use of CA-loaded polymeric nanoparticles to improve the antitumor activity of breast cancer cells (MCF-7) and colon cancer cells (Caco-2). CA was encapsulated in bovine serum albumin (BSA), chitosan (CH), and cellulose (CL) nanoparticles. The CA-loaded BSA nanoparticles (CA-BSA-NPs) revealed the most promising formula as it showed good loading capacity and the best release rate profile as the drug reached 80% after 10 h. The physicochemical characterization of the CA-BSA-NPs and empty carrier (BSA-NPs) was performed by the particle size distribution analysis, transmission electron microscopy (TEM), and zeta potential. The antitumor activity of the CA-BSA-NPs was evaluated by measuring cell viability, apoptosis rate, and gene expression of GCLC, COX-2, and BCL-2 in MCF-7 and Caco-2. The cytotoxicity assay (MTT) showed elevated antitumor activity of CA-BSA-NPs against MCF-7 and Caco-2 compared to free CA and BSA-NPs. Moreover, apoptosis test data showed an arrest of the Caco-2 cells at G₂/M (10.84%) and the MCF-7 cells at G2/M (4.73%) in the CA-BSA-NPs treatment. RT-PCR-based gene expression analysis showed an upregulation of the GCLC gene and downregulation of the BCL-2 and COX-2 genes in cells treated with CA-BSA-NPs compared to untreated cells. In conclusion, CA-BSA-NPs has been introduced as a promising formula for treating breast and colorectal cancer.     

The Intestinal and Biliary Metabolites of Ibuprofen in the Rat with Experimental Hyperglycemia

Hyperglycemia is reported to be associated with oxidative stress. It can result in changes in the activities of drug-metabolizing enzymes and membrane-integrated transporters, which can modify the fate of drugs and other xenobiotics; furthermore, it can result in the formation of non-enzyme catalyzed oxidative metabolites. The present work aimed to investigate how experimental hyperglycemia affects the intestinal and biliary appearance of the oxidative and Phase II metabolites of ibuprofen in rats. In vivo studies were performed by luminal perfusion of 250 μM racemic ibuprofen solution in control and streptozotocin-treated (hyperglycemic) rats. Analysis of the collected intestinal perfusate and bile samples was performed by HPLC-UV and HPLC-MS. No oxidative metabolites could be detected in the perfusate samples. The biliary appearance of ibuprofen, 2-hydroxyibuprofen, ibuprofen glucuronide, hydroxylated ibuprofen glucuronide, and ibuprofen taurate was depressed in the hyperglycemic animals. However, no specific non-enzymatic (hydroxyl radical initiated) hydroxylation product could be detected. Instead, the depression of biliary excretion of ibuprofen and ibuprofen metabolites turned out to be the indicative marker of hyperglycemia. The observed changes impact the pharmacokinetics of drugs administered in hyperglycemic individuals.     

Simultaneous Estimation of Escitalopram and Clonazepam in Tablet Dosage Forms Using HPLC-DAD Method and Optimization of Chromatographic Conditions by Box-Behnken Design

The study aimed to develop a new reverse-phase high-performance liquid chromatography (RP-HPLC) method with diode array detection (DAD) detection for simultaneous estimation of escitalopram (EST) and clonazepam (CZP) in tablet dosage forms with a quality by design (QbD) approach. The chromatographic conditions were optimized by Box-Behnken design (BBD) and developed method was validated for the linearity, system suitability, accuracy, precision, robustness, sensitivity, and solution stability according to International Council for Harmonization (ICH) guidelines. EST and CZP standard drugs peaks were separated at retention times of 2.668 and 5.046 min by C-18 column with dimension of 4.6 × 100 mm length and particle size packing 2.5 µm. The mobile phase was methanol: 0.1% orthophosphoric acid (OPA) (25:75, v/v), with a flow rate of 0.7 mL/min at temperature of 26 °C. The sample volume injected was 20 µL and peaks were detected at 239 nm. Using the standard calibration curve, the % assay of marketed tablet was founded 98.89 and 98.76 for EST and CZP, respectively. The proposed RP-HPLC method was able to detect EST and CZP in the presence of their degradation products, indicating the stability-indicating property of the developed RP-HPLC method. The validation parameter’s results in terms of linearity, system suitability, accuracy, precision, robustness, sensitivity, and solution stability were in an acceptable range as per the ICH guidelines. The newly developed RP-HPLC method with QbD application is simple, accurate, time-saving, and economic.     

Sarcorucinine-D Inhibits Cholinesterases and Calcium Channels: Molecular Dynamics Simulation and In Vitro Mechanistic Investigations

Acetylcholinesterase (AChE) inhibitors and calcium channel blockers are considered effective therapies for Alzheimer’s disease. AChE plays an essential role in the nervous system by catalyzing the hydrolysis of the neurotransmitter acetylcholine. In this study, the inhibition of the enzyme AChE by Sarcorucinine-D, a pregnane type steroidal alkaloid, was investigated with experimental enzyme kinetics and molecular dynamics (MD) simulation techniques. Kinetics studies showed that Sarcorucinine-D inhibits two cholinesterases—AChE and butyrylcholinesterase (BChE)—noncompetitively, with K_i values of 103.3 and 4.66 µM, respectively. In silico ligand-protein docking and MD simulation studies conducted on AChE predicted that Sarcorucinine-D interacted via hydrophobic interactions and hydrogen bonds with the residues of the active-site gorge of AChE. Sarcorucinine-D was able to relax contractility concentration-dependently in the intestinal smooth muscles of jejunum obtained from rabbits. Not only was the spontaneous spasmogenicity inhibited, but it also suppressed K⁺-mediated spasmogenicity, indicating an effect via the inhibition of voltage-dependent Ca²⁺ channels. Sarcorucinine-D could be considered a potential lead molecule based on its properties as a noncompetitive AChE inhibitor and a Ca²⁺ channel blocker.