Preparation and characterization of Cu (II) supported on poly(8‐hydroxyquinoline‐p‐styrene sulphonate) and its application as catalyst for the synthesis of hexahydroquinolines

Cu ( II ) supported on poly(8‐hydroxyquinoline‐p‐styrenesulfonate) (Cu ( II )@PHQSS) was prepared and fully characterized by the different techniques including fourier transform infrared spectroscopy (FT‐IR), ¹H NMR, ¹³C NMR, thermal gravimetric analysis (TGA), differential thermal gravimetric (DTG), differential thermal analysis (DTA), scanning electron microscope (SEM) and energy dispersive X‐ray analysis (EDS). Afterward, the Cu ( II )@PHQSS as nanostructured catalyst was used as catalyst for the synthesis of hexahydroquinolines.     

Effect of deuteron density distribution on the deduction of screening potential from the D(d,p)T reaction in Be metals

The D(d,p)T reaction in Be metal environments has been measured to investigate the electron screening effect in metals in an energy region of from 5.5 keV to 10 keV in a center of mass system(CMS)at a temperature of 121 K.The depth distribution of deuteron density in Be metals has an impact on the observed reaction yields.A model of deuteron density distribution in metal has been proposed to obtain the original yields.A screening energy of(116±46)eV has been obtained with the assumed deuteron density distribution model.     

The structure of glibenclamide in the solid state

The structure of glibenclamide, 5‐chloro‐N‐(2‐{4‐[(cyclohexylamino)carbonyl] aminosulfonyl}phenyl) ethyl)‐2‐methoxybenzamide, an important antidiabetic drug, has been studied both in solution and in the solid state by a combination of NMR spectroscopy and theoretical calculations. The possibility that glibenclamide suffers a tautomerization under melting to afford a desmotrope was rejected. Copyright © 2012 John Wiley & Sons, Ltd.     

Preparation,characterization, biological activity,density functional theory calculations and molecular docking of chelates of diazo ligand derived from m‐phenylenediamine and p‐chlorophenol

A novel azo dye ligand, 2,2′‐(1,3‐phenylenebis(diazene‐2,1‐diyl))bis(4‐chlorophenol), was synthesized from the diazotization of m ‐phenelyenediamine and coupling with p ‐chlorophenol in alkaline medium. Mononuclear Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes of the azo ligand (H₂L) were prepared and characterized using elemental analyses, infrared spectroscopy, electron spin resonance, magnetic susceptibility, conductance measurements and thermal analyses. The UV–visible, ¹H NMR and mass spectra of the ligand and its chelates were also recorded. The analytical data showed that the metal‐to‐ligand ratio in the mononuclear azo complexes was 1:1. Diffuse reflectance and magnetic moment measurements revealed the complexes to have octahedral geometry. The infrared spectral data showed that the chelation behaviour of the ligand towards transition metal ions was through phenolic oxygen and azo nitrogen atoms. The electronic spectral results indicated the existence of π → π* (phenyl rings) and n → π* (─N═N) and confirmed the mentioned structure. Molar conductivity revealed the non‐electrolytic nature of all chelates. The presence of water molecules in all complexes was supported by thermal studies. Molecular docking was used to predict the binding between H₂L and the receptors of breast cancer mutant 3hb5‐oxidoreductase, crystal structure of Escherichia coli (3 t88) and crystal structure of Staphylococcus aureus (3q8u). The molecular and electronic structure of H₂L was optimized theoretically and the quantum chemical parameters were calculated. In addition, the effects of the H₂L azo ligand and its complexes on the inhibition of bacterial or fungal growth were evaluated. The prepared complexes had enhanced activity against bacterial or fungal growth compared to the H₂L azo ligand.     

Separation and Analysis of o.p'-DDD and its Lipophilic Metabolite,O.P'-DDE,in Tissue,Faeces and Plasma

Abstract

An analytical procedure based on electron capture gas chromatography for the determination of o,p′-DDD, a drug used for the treatment of Cushing′s syndrome, is presented. Detection of a metabolite, identified as o,p′-DDE, is also described.     

Simultaneous determination of residues of metalaxyl,cyazofamid and a cyazofamid metabolite in tobacco leaves and soil by liquid chromatography with tandem mass spectrometry

A simple method was developed and validated for the simultaneous determination of metalaxyl, cyazofamid and the cyazofamid metabolite 4‐chloro‐5‐p‐tolylimidazole‐2‐carbonitrile (CCIM) by liquid chromatography with tandem mass spectrometry. The three target compounds were extracted from tobacco and soil with acetonitrile containing 0.1% acetic acid, and the extracts were purified using octadecylsilane. The proposed method showed satisfactory linearity (R² ≥ 0.9985) for the target compounds. The limits of detection for metalaxyl, cyazofamid and CCIM were 0.006, 0.06 and 0.06 mg/kg in soil and green tobacco leaves and 0.03, 0.3 and 0.3 mg/kg in cured tobacco leaves, respectively. The limits of quantification for metalaxyl, cyazofamid and CCIM were 0.02, 0.2 and 0.2 mg/kg in soil and green tobacco leaves and 0.1, 1 and 1 mg/kg in cured tobacco leaves, respectively. The average recoveries from soil and tobacco were 72.91–98.40% for metalaxyl, 76.73–105.80% for cyazofamid and 74.48–106.45% for CCIM. The relative standard deviation range was 1.23–6.99%. The developed method was successfully applied to analysis of residues of metalaxyl, cyazofamid and CCIM in real soil and tobacco samples. The results indicated that the established method could meet the requirement for the analysis of trace amounts of all three analytes in soil and tobacco.     

Biological and catalytic evaluation of Ru(II)‐p‐cymene complexes of Schiff base ligands: Impact of ligand appended moiety on photo‐induced DNA and protein cleavage,cytotoxicity and C‐H activation

Two organometallic Ru(II)‐p‐cymene complexes of the type [Ru(η⁶‐p‐cymene)(L)Cl]PF₆ 1 and 2 , where L is N,N‐bis(4‐isopropylbenzylidene)ethane‐1,2‐diamine (bien, L1 ) or N,N‐bis (pyren‐2‐ylmethylene)ethane‐1,2‐diamine (bpen, L2 ) have been prepared and characterized well. Because of appended pyrenyl groups in coordinated bpen ligand, the complex 2 exhibits higher DNA and protein binding than complex 1 in which isopropylbenzyl groups are incorporated. Interestingly, the luminescent characteristic complex 2 is unique in displaying DNA cleavage after light activation by UVA light at 365 nm through oxygen dependent mechanism. AFM analysis attests the photo‐induced DNA fragmentation ability of complex 2 . Also, the complex 2 cleaves the protein after light exposure in a non‐specific manner suggesting that it can act as a protein photo cleaving agent. In contrast to the trend of DNA and protein interaction of complexes, the complex 1 exhibits cytotoxic activity against human breast carcinoma ( MCF‐7 ) and liver carcinoma ( HepG2 ) with potency higher than that of complex 2 due to enhanced hydrophobicity of isopropyl groups present in p‐cymene and bien ligands. Indeed, complex 2 is inactive against MCF‐7 and HepG2 cancer cell lines even up to 200 μM concentration. The AO/EB staining assay reveals that the complex 1 is able to induce late apoptotic mode of cell death in breast cancer cells, which is further confirmed by inter‐nucleosomal DNA cleavage. Furthermore, the complexes 1 and 2 are evaluated for their catalytic activities and found to be working well for the β‐carboline directed C–H arylation to afford the desired products in good yield (40–47%).     

Effect of Butyric Acid on p53 Expression and Apoptosis in Colon Epithelial Cells in Mice after Treated with 9,10-dimethyl-1,2-benz(a)anthracene

As the most common cancer, colorectal cancer is the fourth leading cause of death among this malignancy disease. Surgery procedure with chemotherapy and radiotherapy for colorectal cancer treatment may cause unpleasant side effects. Therefore, prevention and early detection of the disease is important. Butyrate, a short chain fatty acid, has a protective effect against colon cancer by inhibiting cell proliferation and inducing apoptosis. We conduct a research to investigate the effect of butyrate as a possible agent to decreased mutant p53 gene expression.