Synthesis and Anticancer Activity of Certain Selenophene Derivatives

Russian Journal of Organic Chemistry - Selenopheno[2,3-d]pyrimidine- and selenopheno[2,3-d][1,2,3]triazine-containing compounds were synthesized starting from...     

A Biosilification Fusion Protein for a ‘Self‐immobilising’ Sarcosine Oxidase Amperometric Enzyme Biosensor

Monomeric sarcosine oxidase (mSOx) fusion with the silaffin peptide, R5, designed previously for easy protein production in low resource areas, was used in a biosilification process to form an enzyme layer electrode biosensor. mSOx is a low activity enzyme (10–20 U/mg) requiring high amounts of enzyme to obtain an amperometric biosensor signal, in the clinically useful range <1 mM sarcosine, especially since the K_m is >10 mM. An amperometric biosensor model was fitted to experimental data to investigate dynamic range. mSOx constructs were designed with 6H (6×histidine) and R5 (silaffin) peptide tags and compared with native mSOx. Glutaraldehyde (GA) cross‐linked proteins retained ～5 % activity for mSOx and mSOx‐6H and only 0.5 % for mSOx‐R5. In contrast R5 catalysed biosilification on (3‐mercaptopropyl) trimethoxysilane (MPTMS) and tetramethyl orthosilicate (TMOS) particles created a ‘self‐immobilisation’ matrix retaining 40 % and 76 % activity respectively. The TMOS matrix produced a thick layer (>500 μm) on a glassy carbon electrode with a mediated current due to sarcosine in the clinical range for sarcosinemia (0–1 mM). The mSOx‐R5 fusion protein was also used to catalyse biosilification in the presence of creatinase and creatininase, entrapping all three enzymes. A mediated GC enzyme linked current was obtained with dynamic range available for creatinine determination of 0.1–2 mM for an enzyme layer ～800 nm.     

A novel synthesis route for brookite rich titanium dioxide photocatalyst involving organic intermediate

Journal of Sol-Gel Science and Technology - High temperature stable brookite rich titanium dioxide of average crystallite size 20&;nbsp;nm has been prepared by a novel aqueous sol–gel...     

Optimized spacer layer thickness for plasmonic-induced enhancement of photocurrent in a-Si:H

Journal of Nanoparticle Research - Plasmonic interfaces consisting of silver nanoparticles of different sizes (50–100&;nbsp;nm) have been processed by the self-assembled dewetting...     

Formation and pharmacological activity of silicon—chitosan-containing glycerohydrogels obtained by biomimetic mineralization

The biomimetic sol—gel synthesis of silicon—chitosan-containing glycerohydrogels was carried out using silicon tetraglycerolate as a precursor. It was found that chitosan accelerates gel formation in weakly acidic media. In more acidic media, the kinetics of the process changes according to the curve with a maximum, which can be attributed to different mechanisms of silanol condensation before and after the isoelectric point. The investigated silicon—chitosan-containing glycerohydrogels exhibit antibacterial, anti-inflammatory, and wound healing activity. The synthesized hybrid glycerohydrogels are promising materials for biomedical applications.     

Separation and analysis of triazine herbcide residues by capillary electrophoresis

Triazines are widely used in agriculture around the world as selective pre‐ and post‐emergence herbicides for the control of broad leaf and grassy weeds. With high toxicity and persistence, triazines can contaminate the environment and crops, so the development of rapid and sensitive methods for the determination of different triazines is necessary. Capillary electrophoresis comprises a group of techniques used to separate chemical mixtures. Analytical separation is based on different electrophoretic mobilities. This review focuses on the analysis of triazine herbicides with different modes of capillary electrophoresis, including capillary zone electrophoresis, micellar electrokinetic capillary electrophoresis, capillary electrochromatography and nonaqueous capillary electrophoresis. Determinations of triazines in various matrices such as surface water, groundwater, vegetables, soil and grains are emphasized. Copyright © 2014 John Wiley & Sons, Ltd.     

A volatolomic approach using cerumen as biofluid to diagnose bovine intoxication by Stryphnodendron rotundifolium

An innovative volatolomic approach employs the detection of biomarkers present in cerumen (earwax) to identify cattle intoxication by Stryphnodendron rotundifolium Mart., Fabaceae (popularly known as barbatimão). S. rotundifolium is a poisonous plant with the toxic compound undefined and widely distributed throughout the Brazilian territory. Cerumen samples from cattle of two local Brazilian breeds (‘Curraleiro Pé-Duro’ and ‘Pantaneiro’) were collected during an experimental intoxication protocol and analyzed using headspace (HS)/GC–MS followed by multivariate analysis (genetic algorithm for a partial least squares, cluster analysis, and classification and regression trees). A total of 106 volatile organic metabolites were identified in the cerumen samples of bovines. The intoxication by S. rotundifolium influenced the cerumen volatolomic profile of the bovines throughout the intoxication protocol. In this way, it was possible to detect biomarkers for cattle intoxication. Among the biomarkers, 2-octyldecanol and 9-tetradecen-1-ol were able to discriminate all samples between intoxicated and nonintoxicated bovines. The cattle intoxication diagnosis by S. rotundifolium was accomplished by applying the cerumen analysis using HS/GC–MS, in an easy, accurate, and noninvasive way. Thus, the proposed bioanalytical chromatography protocol is a useful tool in veterinary applications to determine this kind of intoxication.     

The 1H and 13C NMR chemical shifts of Strychnos alkaloids revisited at the DFT level

The density functional theory calculation of ¹H and ¹³C NMR chemical shifts in a series of ten 10 classically known Strychnos alkaloids with a strychnine skeleton was performed at the PBE0/pcSseg-2//pcseg-2 level. It was found that calculated ¹H and ¹³C NMR chemical shifts provided a markedly good correlation with experiment characterized by a mean absolute error of 0.08 ppm in the range of 7 ppm for protons and 1.67 ppm in the range of 150 ppm for carbons, so that a mean absolute percentage error was as small as ~1% in both cases.     

Identifying aspirin polymorphs from combined DFT-based crystal structure prediction and solid-state NMR

A combined experimental and computational approach was used to distinguish between different polymorphs of the pharmaceutical drug aspirin. This method involves the use of ab initio random structure searching (AIRSS), a density functional theory (DFT)-based crystal structure prediction method for the high-accuracy prediction of polymorphic structures, with DFT calculations of nuclear magnetic resonance (NMR) parameters and solid-state NMR experiments at natural abundance. AIRSS was used to predict the crystal structures of form-I and form-II of aspirin. The root-mean-square deviation between experimental and calculated ¹H chemical shifts was used to identify form-I as the polymorph present in the experimental sample, the selection being successful despite the large similarities between the molecular environments in the crystals of the two polymorphs.