Determination of isoniazid and hydrazine by capillary electrophoresis with amperometric detection at a Pt-particle modified carbon fiber microelectrode

Capillary electrpphoresis (CE)/electrochemical detection (EC) for the simultane-ous determination of hydrazine and isoniazid has been developed.The electrochemical method uses a novel modified electrode dispersed with ultrafine platinum particles on the surface of a 30μm carbon fiber microelectrode.The unique characteristic of the Pt-particles modified carbon fiber microelectrode is its excellent stability.The current measurement for hydrazine is more sensitive than that of isoniazid.Selective determination of trace amount of free hydrazine in isoniazid and its formulation can be achieved at applied potential of 0.5V.     

Facile synthesis, structure, and properties of benzo[1,2-b:4,5-b']dichalcogenophenes

[reaction, structures: see text] A general and convenient synthesis of benzo[1,2-b:4,5-b']dichalcogenophenes including the thiophene (BDT, 1), selenophene (BDS, 2), and tellurophene (BDTe, 3) homologues is developed. Thus synthesized heterocycles are structurally characterized by single-crystal X-ray analysis, and all three homologues are isostructural with one another. They all have completely planar molecular structures packed in a herringbone arrangement. Their physicochemical properties were also elucidated by means of cyclic voltammetry (CV) and UV-vis spectra.     

Near-infrared absorbing Ru(ii) complexes act as immunoprotective photodynamic therapy (PDT) agents against aggressive melanoma

Mounting evidence over the past 20 years suggests that photodynamic therapy (PDT), an anticancer modality known mostly as a local treatment, has the capacity to invoke a systemic antitumor immune response, leading to protection against tumor recurrence. For aggressive cancers such as melanoma, where chemotherapy and radiotherapy are ineffective, immunomodulating PDT as an adjuvant to surgery is of interest. Towards the development of specialized photosensitizers (PSs) for treating pigmented melanomas, nine new near-infrared (NIR) absorbing PSs based on a Ru(ii) tris-heteroleptic scaffold [Ru(NNN)(NN)(L)]Cl_n, were explored. Compounds 2, 6, and 9 exhibited high potency toward melanoma cells, with visible EC₅₀ values as low as 0.292–0.602 μM and PIs as high as 156–360. Single-micromolar phototoxicity was obtained with NIR-light (733 nm) with PIs up to 71. The common feature of these lead NIR PSs was an accessible low-energy triplet intraligand (³IL) excited state for high singlet oxygen (¹O₂) quantum yields (69–93%), which was only possible when the photosensitizing ³IL states were lower in energy than the lowest triplet metal-to-ligand charge transfer (³MLCT) excited states that typically govern Ru(ii) polypyridyl photophysics. PDT treatment with 2 elicited a pro-inflammatory response alongside immunogenic cell death in mouse B16F10 melanoma cells and proved safe for in vivo administration (maximum tolerated dose = 50 mg kg⁻¹). Female and male mice vaccinated with B16F10 cells that were PDT-treated with 2 and challenged with live B16F10 cells exhibited 80 and 55% protection from tumor growth, respectively, leading to significantly improved survival and excellent hazard ratios of ≤0.2.

Ru(ii) photosensitizers (PSs) destroy aggressive melanoma cells, triggering an immune response that leads to protection against tumor challenge and mouse survival.     

Reactivity of ketene dithiolates toward alkyl bromides

The reactivity of barbituric/thiobarbituric ketene dithiolates with bromoacetic ester and phenacyl bromide is studied. J. Heterocyclic Chem., (2011).     

A convenient approach to total synthesis of synargentolide-B from l-ascorbic acid and d-ribose

A convenient and practical approach for the total synthesis of naturally occurring lactone synargentolide-B has been accomplished in 14 steps from the commercially available l-ascorbic acid and d-ribose involving Bestmann–Ohira reaction, zinc mediated allylation, ring closing-metathesis, and cross-metathesis reactions. The highlight of our strategy describes a one-pot reaction involving stereoselective addition of allylzinc reagent and selective reduction of terminal alkyne to obtain the key advanced intermediates.     

Reduction of core loss in non-oriented (NO) electrical steel by electroless-plated magnetic coating

An important issue in development of electrical steels for core-laminated products is to reduce core loss to improve energy conversion efficiency. This is usually obtained by tailoring the composition, microstructure, and texture of electrical steels themselves. A new technique to reduce core loss in electrical steel has been investigated. This technique involves electroless plating of magnetic thin coating onto the surface of electrical steel. The material system was electroless Ni–Co–P coatings with different thicknesses (1, 5, and 10 μm) deposited onto the surface of commercially available Fe–3% Si electrical steel. Characterization of deposited Ni–Co–P coating was carried out using X-ray diffraction (XRD), scanning electron microscope (SEM), and energy dispersive X-ray (EDX) spectrometer. The deposited Ni–Co–P coatings were amorphous and composed of 56–59% Ni, 32–35% Co, and 8–10% P by mass. The effect of coatings on core loss of the electrical steel was determined using single sheet test. A core loss reduction of 4% maximum was achieved with the Ni–Co–P coating of 1 μm thickness at 400 Hz and 0.3 T.     

Inhibition of Insulin-Regulated Aminopeptidase (IRAP) by Arylsulfonamides

The inhibition of insulin-regulated aminopeptidase (IRAP, EC 3.4.11.3) by angiotenesin IV is known to improve memory and learning in rats. Screening 10 500 low-molecular-weight compounds in an enzyme inhibition assay with IRAP from Chinese Hamster Ovary (CHO) cells provided an arylsulfonamide (N-(3-(1H-tetrazol-5-yl)phenyl)-4-bromo-5-chlorothiophene-2-sulfonamide), comprising a tetrazole in the meta position of the aromatic ring, as a hit. Analogues of this hit were synthesized, and their inhibitory capacities were determined. A small structure–activity relationship study revealed that the sulfonamide function and the tetrazole ring are crucial for IRAP inhibition. The inhibitors exhibited a moderate inhibitory potency with an IC₅₀=1.1±0.5 μm for the best inhibitor in the series. Further optimization of this new class of IRAP inhibitors is required to make them attractive as research tools and as potential cognitive enhancers.     

Investigating the vortex melting phenomenon in BSCCO crystals using magneto-optical imaging technique

Using a novel differential magneto-optical imaging technique we investigate the phenomenon of vortex lattice melting in crystals of Bi₂Sr₂CaCu₂O₈ (BSCCO). The images of melting reveal complex patterns in the formation and evolution of the vortex solid-liquid interface with varying field (H)/temperature (T). We believe that the complex melting patterns are due to a random distribution of material disorder/inhomogeneities across the sample, which create fluctuations in the local melting temperature or field value. To study the fluctuations in the local melting temperature/field, we have constructed maps of the melting landscape T _m(H, r), viz., the melting temperature (T _m) at a given location (r) in the sample at a given field (H). A study of these melting landscapes reveals an unexpected feature: the melting landscape is not fixed, but changes rather dramatically with varying field and temperature along the melting line. It is concluded that the changes in both the scale and shape of the landscape result from the competing contributions of different types of quenched disorder which have opposite effects on the local melting transition.