Synthesis,characterization and biological analysis of transition metal complexes with macro cyclic ligands derived from adipic acid,ethylenediamine with diethyloxalate and diethylmalonate

Macro-cyclic ligands from adipic acid, ethylenediamine with diethyloxalate and diethylmalonate and their respective metal complexes of Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) with macro cyclic ligands (LO) and (LM) L [N,N′-bis(2-aminoethyl)hexanediamide] were synthesized successfully. These metal complexes were characterized by Fourier transform infrared, ultraviolet visible spectrometry, proton nuclear magnetic resonance spectroscopy, and mass Spectrometry, CHNS and thermogravimetric analysis. The elemental analysis confirms the structures for Mn(II), Co(II) and Ni(II) complexes similar to octahedral geometry, Cu(II) complexes as a square planar geometry and Zn(II) complexes in the tetrahedral geometry. The molar conductivities of all the metal complexes were taken in 10^?3 M DMSO, and values of all the metal complexes showed their electrolytic nature which indicates the presence of chloride ions. Thermal analysis supports as the metal complexes are thermally stable. The result of antimicrobial activity against various microorganisms confirms that the metal complexes are potent bactericides and fungicides than the ligand. Metal complexes of LO with Cu(II) and Zn(II) were found to be highly active against S. typhimurium than the complexes of LM.

Graphical abstract

Open image in new window

     

Cytotoxicity,In vitro anti-Leishmanial and fingerprint HPLC- photodiode array analysis of the roots of Trillium govanianum

Trillium govanianum Wall. ex D. Don (Melanthiaceae alt. Trilliaceae), commonly known as ‘nagchhatry’ or ‘teen patra’, distributed from Pakistan to Bhutan about 2500–3800 m altitude is indigenous to Himalayas region. In folk medicine the plant has been reported for the treatment of wound healing, sepsis and in various sexual disorders. This paper reports, for the first time, to evaluate the cytotoxicity, in vitro anti-leishmanial (promastigotes) and fingerprint HPLC-photodiode array analysis of the MeOH extract of the roots of T. govanianum and its solid phase extraction fractions. Reverse phase HPLC-PDA based quantification revealed the presence of significant amount of quercetin, myrecetin and kaemferol ranging from 0.221to 0.528 μg/mg DW. MeOH extract revealed distinguishable protein kinase inhibitory activity against Streptomyces 85E strain with 18 mm bald phenotype. The remarkable toxicity profile against brine shrimps and leishmanial was manifested by MeOH extract with LC₅₀ 10 and 38.5 μg/mL, respectively.     

Density functional theory assessment of the thermal degradation of diclofenac and its calcium and iron complexes

Thermogravimetric analyses of diclofenac sodium, its Ca²⁺ and Fe³⁺ complexes manifested a decreasing trend of the onset decomposition temperatures at which these compounds dissociated. The drop in the temperature was metal ion dependent; the sodium salt showed thermal stability up to 245 °C, whereas the complexes started their degradation processes at temperatures starting from 90 °C. While G* for the cleavage of the acetate moiety in the sodium salt was 63.76 kJmol⁻¹, it was 82.06 and 140.57 kJmol⁻¹ in the cases of Ca²⁺ and Fe³⁺, respectively. However, their complete fusion took place at 187.65, 150.34 and 98.77 °C, respectively, displaying a reversed trend which is probably indicative of some catalytic part on the binding metals.

Using the Gaussian 98 W package of programs, ab initio molecular orbital treatments were applied to diclofenac and its Ca²⁺ and Fe³⁺ metal complexes to study their electronic structure at the atomic level. The thermochemistry of diclofenac sodium was followed through the TG fragmentation peak temperatures using the density functional theory calculations at the 6-31G(d) basis set level. The FT-IR data were in good agreement with the theoretically calculated values.

Single point calculations at the B3LYP/ 6-311G(d) level of theory, were used to compare the geometric features, energies and dipole moments of these compounds to detect the effect of the binding metal ions on the thermal dissociation of their diclofenac complexes.     

Iridoid glycosides from Globularia davisiana

From the ethanolic extract of the aerial parts of Globularia davisiana, a new iridoid glycoside, davisioside (1), was isolated. Davisioside (1) comprises a rare iridoid aglycone structure with a saturated double bond between C-3 and C-4. Nine known iridoid glycosides, asperuloside (2), alpinoside (3), geniposide (4), globularin (5), globularicisin (6), 10-O-benzoylcatalpol (7), lytanthosalin (8), melampyroside (9), agnuside (10), and three known phenylethanoid glycosides, verbascoside, isoacteoside and leucosceptoside A were also isolated and characterized. The structures of the isolates were established by spectroscopic methods (one-dimensional (1D)- and two-dimensional (2D)-NMR, MS).     

Estimation of Residual Nickel and Some Heavy Metals in Vanaspati Ghee

To convert vegetable edible oils into vanaspati ghee, nickel is used as a catalyst in the hydrogenation process. A simple and fast method for the trace level determination of nickel in ghee is reported. In this work different methods were applied for the extraction of residual nickel from ghee samples. Using toluene, benzene and carbon tetrachloride as organic solvents, an acid mixture was used for the extraction of nickel. Extracted nickel was quantified with atomic absorption and colorimetric methods. Among the organic solvents, toluene proved to be the best solvent mediating a 95% extraction of nickel from ghee samples. Nickel was extracted and determined in ten different brands of ghee and in all samples its amount was well above the permissible limit of WHO (0.2 μg/g). Other metals like lead, zinc, copper, and cadmium were also determined and their concentrations were found to be much below the WHO permissible limits.     

Lucidin type anthraquinone glycosides from Putoria calabrica

Two new lucidin type anthraquinone glycosides, putorinoside A (1) and putorinoside B (2) were isolated from Putoria calabrica, in addition to two known anthraquinone glycosides, lucidin 3-O-beta-glucopyranoside (3) and lucidin 3-O-primeveroside (4). Based on spectroscopic data, putorinosides A and B were identified as 2-hydroxymethyl-1-methoxy-3,5,6-trihydroxyanthraquinone 3-O-beta-glucopyranoside and 2-hydroxymethyl-1-methoxy-3,6-dihydroxyanthraquinone 3-O-beta-glucopyranoside, respectively.     

Ensemble average of an arbitrary number of pairs of different eigenvalues using Grassmann integration

An identity satisfied by the eigenvalues of a real-symmetric matrix and an integral representation of a determinant using Grassmann variables are used to show that the ensemble average ofS different pairs of eigenvalues of a GOE is given by (–1) ^S 2^{–S –1/2}(S+1/2).     

Darstellung und schwingungsspektren von trimethylzinndiorganothiophosphinaten Me3SnOSPR′R″ (R′R″ = Me2, MePh,Ph2). Die kristallstruktur von Me3SnOSPMe2

A series of trimethyltin diorganothiophosphinates Me₃SnOSPR′R″ (R′R″ = Me₂, MePh, Ph₂) was prepared from (Me₃Sn)₂O and R′R″PSCl in cyclohexane solution. A close study of the vibrational spectra is given; ³¹P NMR and mass spectra are also reported. The structural investigation of Me₃SnOSPMe₂ by means of X-ray diffraction (R 5.2%, 1697 observed independent reflexions) shows the compound to consists of chains, in which planar SnMe₃ units and tetrahedral OSPMe₂ groups are linked by the O- and S-atoms of the thiophosphinate.     

Spectrophotometric Determination of Prochlorperazine Maleate in Pure and Pharmaceutical Preparations

 Prochlorperazine maleate reacts with 1-naphthylamine and sodium nitrite, after heating for 110 s at 80 °C to give an orange red colour having maximum absorbance at 460 nm. The reaction is selective for prochlorperazine maleate with 0.01 mg/mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.01 mg/10 mL to 0.33 mg/10 mL of prochlorperazine maleate and the relative standard deviation is 0.68%. The quantitative assessment of tolerable amounts of other drugs is also studied. Received September 22, 2000. Revision June 19, 2001     

2020 Roadmap on gas-involved photo-and electro-catalysis

In this roadmap, we address the development and perspectives of hydrogen evolution reaction, oxygen reduction reaction, oxygen evolution reaction, carbon dioxide reduction reaction and nitrogen reduction.