Synthesis of the dicyanopentasulfidonickelate(II) anion

Potassium tetracyanonickelate reacts with elemental sulfur and KOH in DMF to give the [(NC)₂NiS₅]^2? anion, which has been isolated as its PPh₄⁺ and AsPh₄⁺ salts. The XPS S(2p) binding energies of the S₅ ring sulfur are in the ratio 2(162.8 eV)/3(163.6 eV). Cyclic voltammetry shows that the compound undergoes an irreversible reduction at ?1.825 V.     

Regioselective oxidation of N-alkylpyrrolidines to pyrrolidin-5-ones by RuCl3/NaIO4

RuCl₃/NaIO₄ under EtOAc/H₂O biphasic conditions, selectively oxidizes the Nα-endo-methylene group of pyrrolidine derivatives, without affecting the exo-methylene group adjacent to the N-heteroatom.     

Synthesis, characterization and antitumour studies on N-salicyl-N′-thiobenzohydrazide and its copper(II) complex

Summary The new potential tetradentate ligand N-salicyl-N-thiobenzohydrazide (H₂SBTH) and its Cu complex, [Cu(SBTH)], have been prepared and characterized by physico-chemical studies. In vivo antitumour activity of [Cu(SBTH)] has been tested against breast tumour in C₃H/J strain mice; LD ₅₀ values were also calculated. The cytotoxicity and antitumour effect of [Cu(SBTH)] is a maximum at 100 mg kg^-1 body weight injected intraperitoneally in mice carrying breast tumour. In vitro results of the ligand and the complex on P-815 (murine mastocytoma) and K-562 (human erythroleukemia cells) indicate that these compounds show significant inhibition on ³H-thymidine and ³H-uridine incorporation in DNA and RNA in these tumour cells. Light microscopic study of the treated tumour mass demonstrated that certain cellular degradation, such as disappearance of mitotic figures, loss in cellular compactness, distortion of nucleus and disruption of cytoplasmic boundaries, take place in complex-treated mice with tumours.     

Base sequence- and <Emphasis Type="Italic">T</Emphasis><Subscript>m</Subscript>-dependent DNA oligomer separation by open tubular capillary columns carrying complementary DNA oligomers as probes

DNA chips prepared on a flat glass surface have unavoidable drawbacks when used for quantitative analysis. In an attempt to overcome this problem, we constructed an HPLC-type system suitable for quantitative analysis that enables base sequence- and T _m-dependent DNA oligomer separation in a flow system. A small open tubular capillary column (300-mm × 100-μm I.D.) was used. The DNA oligomers used as probes had an amino group at the 5′-end and were immobilized on the inner silica surface of the capillary column which had been sequentially treated with 3-aminopropyltriethoxysilane, butyltrimethoxysilane, and disuccinimidylglutarate. Using the combination of probe-immobilized column placed in a column oven equipped with temperature gradient function, a nano-flow-controllable pump, a small sample-loading injector, and a capillary-fitted UV detector, we succeeded in separating complementary and non-complementary DNA oligomers in specific and quantitative modes. We also designed a temperature gradient strategy for efficient separation of target DNA oligomers in DNA mixture samples. Using a column carrying two different probes with similar T _m values, their complementary target DNA oligomers were also separated and detected. The developed DNA open tubular capillary column system investigated in the present study could be further improved as an alternative tool to DNA chips to be used for the quantitative analysis of DNA or mRNA samples. Kamakshaiah Charyulu Devarayapalli and Seung Pil Pack contributed equally to this paper.     

Indium-mediated alkynylation of Baylis-Hillman acetates: a novel route to 1,4-enynes

Baylis-Hillman acetates undergo smooth alkynylation with aryl-susbstituted iodoalkynes in the presence of indium metal in refluxing dichloromethane to furnish 1,4-enynes in high yields with (E)-stereoselectivity. In the absence of Lewis acid, the reaction follows both S_N2 and S_N2′ pathways affording 1:1 mixtures of 1,4-enynes. Upon addition of 10 mol % of InBr₃, the reaction proceeds preferably in the S_N2′ manner. In the case of adducts derived from acrylonitrile, the corresponding products are obtained in fairly good yields and with (Z)-stereoselectivity.     

TSP aerosol source apportionment in the urban region of the Indian steel city,Rourkela

Steel industries are a major contributor to aerosols in steel cities like Rourkela.We designed an air quality sampling program to characterize total suspended particulate(TSP) aerosol in urban areas of Rourkela and to identify their steel-related and other sources.Monitoring was carried out over 8 h,twice per week from January 2011 to December 2012.Metallic species of TSP aerosols were analyzed using an atomic absorption spectrophotometer;ionic species using the IS 3025 method;and carbonaceous species using a total organic carbon analyzer.Enrichment factor and Spearman’s rank correlation analysis were carried out on compositional data.Significant seasonal variations were observed for TSP with totals in summer>spring>winter>monsoon.Low concentrations during monsoon reflected wet scavenging,while high concentrations during summer were related to wind turbulence and low humidity.The chemical mass balance model CMB8.2 was applied to apportion sources.Particles related to steel production,road dust,and soil were dominant in all seasons.A fertilizer plant was found to contribute particles in summer and monsoon.Wood combustion,diesel exhaust,and liquefied petroleum gas contributed significantly in spring and winter.While diesel exhaust,industrial manufacturing,solid waste burning,cement kilns,and construction were found to contribute to TSP at various times throughout the year.     

Analogue Implementation of the Funnel Controller

In many tracking control problems, pre-specified bounds for the evolution of the tracking error should be met. The ‘funnel controller’ addresses this requirement and guarantees transient performance for a fairly large class of systems. In addition, only structural assumptions on the underlying system are made; the exact knowledge of the system parameters is not required. This is in contrast to most classical controllers where only asymptotic behaviour can be guaranteed and the system parameters must be known or estimated. Until now, the funnel controller was only studied theoretically. We will present the results of an analogue implementation of the funnel controller. The results show that the funnel controller works well in reality, i.e. it guarantees the pre-specified error bounds. The implementation is an analogue circuit composed of standard devices and is therefore suitable for a broad range of applications. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Study on the Synthesis of ZnO Nanoparticles Using Azadirachta indica Extracts for the Fabrication of a Gas Sensor

This paper compared the effects of A. indica plant proteins over chemical methods in the morphology of zinc oxide nanoparticles (ZnO NPs) prepared by a co-precipitation method, and ethanol sensing performance of prepared thin films deposited over a fluorene-doped tin oxide (FTO) bind glass substrate using spray pyrolysis technique. The average crystallite sizes and diameters of the grain-sized cluster ZnO NPs were 25 and (701.79 ± 176.21) nm for an undoped sample and 20 and (489.99 ± 112.96) nm for A. india dye-doped sample. The fourier transform infrared spectroscopy (FTIR) analysis confirmed the formation of the Zn–O bond at 450 cm⁻¹, and also showed the presence of plant proteins due to A. indica dye extracts. ZnO NPs films exhibited good response (up to 51 and 72% for without and with A. indica dye-doped extracts, respectively) toward ethanol vapors with quick response-recovery characteristics at a temperature of 250 °C for undoped and 225 °C for A. indica dye-doped ZnO thin films. The interaction of A. indica dye extracts helps to decrease the operating temperature and increased the response and recovery rates of the sensor, which may be due to an increase in the specific surface area, resulting in adsorption of more oxygen and hence high response results.     

High-performance thin-layer chromatographic standardization and quantification of marker compounds in an Ayurvedic polyherbal formulation: Krishnadi Churna

JPC – Journal of Planar Chromatography – Modern TLC - The present era is witnessed by the increasing demand for herbal medicine. Therefore, the preparation of herbal drugs is warranted...     

Fluorescent chemosensor for Cu2+ ion based on iminoanthryl appended calix[4]arene

Calix[4]arene based podands 1a of cone conformation and 1b of 1,3-alternate conformation possessing imine units and bearing anthracene moieties have been synthesized by a 1 + 2 Schiff base condensation in good yields and examined for their cation recognition abilities towards cations such as lithium, sodium, potassium, nickel, cadmium, copper, zinc, lead, silver and mercury ions by UV–vis and fluorescence spectroscopy. The calix[4]arene derivative 1b shows a selective fluorescence enhancement in presence of Cu²⁺ ions among the various metal ions tested (Li⁺, Na⁺, K⁺, Ni²⁺, Cd²⁺, Cu²⁺, Zn²⁺, Pb²⁺, Ag⁺ and Hg²⁺ ions). The colour of the solution changes from colourless to light yellow in the presence of Cu²⁺ ions. The stoichiometry of the complex formed between 1b and Cu²⁺ was found to be 1:1 as established by Job’s plot.