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1.
Sci Rep ; 13(1): 9196, 2023 06 06.
Article in English | MEDLINE | ID: mdl-37280267

ABSTRACT

The present investigation goal was to investigate the chemistry of four new mononuclear mixed ligand Fe(III), Co(II), Cu(II), and Cd(II) complexes constructed from furfural-type imine ligand (L), and the co ligand 2,2'-bipyridine in addition to assessing their antimicrobial activity against some bacterial, and fungi strains. The structure of the complexes was interpreted by different spectroscopic techniques such as MS, IR, 1H NMR, UV-Vis, elemental analysis, TG-DTG, conductivity, and magnetic susceptibility measurements. The correlation of all results revealed that ligand (L) acts as a neutral ONNO tetradentate whereas the co ligand acts as a neutral NN bidentate. The coordination of the ligands with the metal ions in a molar ratio of 1:1:1 leads to formation of an octahedral geometry around the metal ions. The octahedral geometry has been validated and optimized by DFT analysis. Conductivity data showed the electrolytic nature of all complexes. The thermal stability of all complexes was deduced in addition to evaluating some thermodynamic, and kinetic parameters using Coats-Redfern method. Furthermore, all complexes in comparison to their parent ligands were tested for their biological potency against some pathogenic bacterial, and fungi strains using the paper disk diffusion method. [CdL(bpy)](NO3)2 complex revealed the highest antimicrobial activity.


Subject(s)
Anti-Infective Agents , Coordination Complexes , Imines , Furaldehyde , Ligands , 2,2'-Dipyridyl/pharmacology , Ferric Compounds , Coordination Complexes/chemistry , Anti-Infective Agents/pharmacology , Anti-Infective Agents/chemistry , Bacteria , Fungi , Ions , Microbial Sensitivity Tests , Spectrophotometry, Infrared , Schiff Bases/chemistry
2.
Heliyon ; 7(1): e06051, 2021 Jan.
Article in English | MEDLINE | ID: mdl-33537484

ABSTRACT

Herein, a simple and accurate spectrophotometric method was developed to detect gatifloxacin (HGAT) in a pure and ophthalmic formulation. The method depends on complexation of HGAT with Co (II), Ni (II) and La(III) ions in ethanol medium at room temperature. The experimental conditions have been investigated to reach optimum conditions for HGAT-metal ions interaction, including detection of a suitable wavelength, medium pH, reaction time and reactants concentration. Moreover, the composition of these complexes in addition to their stability constants were also investigated and the result indicated that the molar ratio of HGAT: Metal ion is 1:1 for Ni (II) and La(III) ions and 1:2 for Co (II) ion. Beer's law plots were obeyed in the concentration ranges 18.77-150.16, 18.77-131.39 and 18.77-112.62 (µg mL-1) for Co(II), Ni(II) and La(III) ions interaction, respectively. The apparent molar absorptivity, Sandell's sensitivity, standard deviation, detection and quantification limits were calculated. The proposed method was successfully applied for the determination of HGAT in the bulk and ophthalmic formulation. The obtained results were compared statistically with other published methods and the results were in good agreement with those obtained by reported methods.

3.
Spectrochim Acta A Mol Biomol Spectrosc ; 105: 109-24, 2013 Mar 15.
Article in English | MEDLINE | ID: mdl-23295217

ABSTRACT

Salicylidene (4-aminotoluene-3-sulfonic acid) Schiff base ligand H(2)L, and its binary and ternary Co(II), Ni(II), Cu(II) and Zn(II) complexes using 8-hydroxyquinoline (8-HOqu) and 2-aminopyridine (2-Ampy) as secondary ligands have been synthesised and characterized via elemental analysis, spectral data (IR, (1)H NMR, mass and solid reflectance), molar conductance, magnetic moment, TG-DSC measurements and XRPD analysis. Correlation of all spectroscopic data suggest that H(2)L ligand acts as monoanionic terdentate ligand with ONO sites coordinating to the metal ions via deprotonated phenolic-O, azomethine-N and sulfonate-O while 2-Ampy behaves as a neutral monodentate ligand via amino group-N and 8-HOqu behaves as a monoanionic bidentate ligand through the ring-N and deprotonated phenolic-O. The thermal behavior of these complexes shows that the coordinated water molecules were eliminated from the complexes at relatively higher temperatures than the hydrated water and there are two routes in removal of coordinated water molecules. All complexes have mononuclear structure and the tetrahedral, square planar or an octahedral geometry have been proposed. The ligand and its complexes have been screened for their antimicrobial activity against Staphylococcus aureus, Bacillus subtilis, Escherichia coli, Salmonella typhimurium, Candida albicans and Aspergillus fumigatus. Among the synthesised compounds, the binary and ternary Ni(II) complexes, (2, 8 and 10) and ternary Zn(II) complex, (12) were found to be very effective against Candida albicans and Bacillus subtilis than all other complexes with MICs of 2 and 8 µg/mL, respectively.


Subject(s)
Anti-Infective Agents/chemistry , Cobalt/chemistry , Copper/chemistry , Nickel/chemistry , Schiff Bases/chemistry , Sulfonic Acids/chemistry , Zinc/chemistry , Aminopyridines/chemical synthesis , Aminopyridines/chemistry , Aminopyridines/pharmacology , Anti-Infective Agents/chemical synthesis , Anti-Infective Agents/pharmacology , Bacteria/drug effects , Bacterial Infections/drug therapy , Cobalt/pharmacology , Coordination Complexes/chemical synthesis , Coordination Complexes/chemistry , Coordination Complexes/pharmacology , Copper/pharmacology , Fungi/drug effects , Humans , Ligands , Mycoses/drug therapy , Nickel/pharmacology , Oxyquinoline/chemical synthesis , Oxyquinoline/chemistry , Oxyquinoline/pharmacology , Schiff Bases/chemical synthesis , Schiff Bases/pharmacology , Spectrum Analysis , Sulfonic Acids/chemical synthesis , Sulfonic Acids/pharmacology , Toluidines/chemical synthesis , Toluidines/chemistry , Toluidines/pharmacology , Zinc/pharmacology
4.
Bioresour Technol ; 101(12): 4446-55, 2010 Jun.
Article in English | MEDLINE | ID: mdl-20185300

ABSTRACT

Rice hulls (RH) and bean hulls (BH) were subjected to prehydrolysis treatments, to define the optimum conditions for producing a high percentage of hydrolyzed hemicellulose with a small or moderate degradation of the cellulosic portion. The hydrolysis experiments were performed using hydrochloric and sulfuric acids in concentrations ranging from (0.5 to 5)% (w/w) at 120 degrees C for 90 min and 10% consistency. The effects of different temperatures (80 to 120 degrees C) and time (30 to 120 min) on acid hydrolysis of lignocellulosic materials were recorded. It was found that, the optimum condition to hydrolyze the lignocellulosic materials (RH) and (BH) are 2% (w/w) of mineral acid at 120 degrees C for 90 min and 10% consistency. The cellulose crystallinity index in the different types of lignocellulosic materials with and without acid treatment, were increased from 0.32 to 0.46 in case of RH and from 0.43 to 0.61 in case of BH. Due to the lignin depolymerization during the pretreatment process, the relative absorbency of the methoxyl group and the aromatic rings bands were lowered for the pretreated than the untreated lignocellulosic materials. Also, the band at 1730 cm(-1) which is attributed to carbonyl groups of uronic acids was lowered due the hemicellulose hydrolysis.


Subject(s)
Acids/pharmacology , Cellulose/chemistry , Lignin/chemistry , Catalysis/drug effects , Fabaceae/chemistry , Hydrolysis/drug effects , Kinetics , Oryza/chemistry , Spectroscopy, Fourier Transform Infrared , Temperature , Thermogravimetry , Time Factors , Water/chemistry , X-Ray Diffraction
5.
Spectrochim Acta A Mol Biomol Spectrosc ; 61(6): 1059-68, 2005 Apr.
Article in English | MEDLINE | ID: mdl-15741103

ABSTRACT

The synthesis and structural characterization of mixed ligand complexes derived from 2,6-pyridinedicarboxaldehydebis(o-hydroxyphenylimine), 2,6-pyridinedicarboxaldehydebis(p-hydroxyphenylimine) (1(ry) ligands) and 2-aminopyridne (2(ry) ligand) are reported. The ligands and their transition metal complexes were characterized on the bases of their elemental analyses, IR, solid reflectance, magnetic moment, molar conductance and thermal analysis (TGA). The mixed ligand complexes are formed in the 1:1:1 (M:L(1) or L(2):L') ratio as found from the elemental analyses and found to have the formulae [MX(2)(L(1) or L(2))(L')].nH(2)O where M = Co(II), Ni(II), Cu(II) and Zn(II), L(1) = 2,6-pyridinedicarboxaldehydebis(p-hydroxyphenylimine), L(2) = 2,6-pyridine dicarboxaldehydebis(o-hydroxyphenylimine), L' = 2-aminopyridine, X = Cl(-) in case of Cu(II) complex and Br(-) in case of Co(II), Ni(II) and Zn(II) complexes and y = 0-3. The molar conductance data reveal that the chelates are non-electrolytes. IR spectra show that the Schiff bases are coordinated to the metal ions in a terdentate manner with NNN donor sites of the pyridine-N and two azomethine-N. While 2-aminopyridine coordinated to the metal ions via its pyridine-N. Magnetic and solid reflectance spectra are used to infer the coordinating capacity of the ligand and the geometrical structure of these complexes are found to be octahedral. The thermal behaviour of these chelates shows that the hydrated water molecules and the anions are removed in a successive two steps followed immediately by decomposition of the ligands (L(1), L(2) and L') in the subsequent steps. The activation thermodynamic parameters, such as, E*, DeltaH*, DeltaS* and DeltaG* are calculated from the TG curves and discussed. The ligands and their metal chelates have been screened for their antimicrobial activities and the findings have been reported, explained and compared with some known antibiotics.


Subject(s)
Anti-Bacterial Agents/chemistry , Anti-Bacterial Agents/pharmacology , Imines/chemistry , Imines/pharmacology , Schiff Bases/chemistry , Schiff Bases/pharmacology , Transition Elements , Anti-Bacterial Agents/chemical synthesis , Chelating Agents/chemical synthesis , Chelating Agents/chemistry , Chelating Agents/pharmacology , Chloramphenicol/pharmacology , Imines/chemical synthesis , Ligands , Microbial Sensitivity Tests , Molecular Structure , Schiff Bases/chemical synthesis , Spectrophotometry, Infrared , Thermodynamics
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