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International Journal of Engineering and Science Invention (IJESI)inventionjournals
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
Synthesis and Characterization of Thermal Analysis of La (Ii) Macrocyclic Com...inventionjournals
The macrocyclic complex compounds of La(II) containing a ligand having tetraoxotetrahydrazin moity are synthesized by template condensation of malonodihydrazide (C3H8N4O2) with different aldehydes. The complexes are characterized on the basis of elemental analysis, UV-visible & IR spectroscopy, magnetic moment and conductance measurement and other physical properties.Antibacterial activity of the derived complex compounds, as well as already used standard compound kanamycin, was tested on fourteen pathogenic bacteria. Given results were then compared to the efficacy of the Antibacterial activity of standard compound kanamycin used for control of these pathogenic bacteria.
SYNTHESIS AND CHARACTERIZATION OF THERMAL ANALYSIS OF La (II) MACROCYCLIC COM...inventionjournals
This document summarizes the synthesis and characterization of lanthanum (II) macrocyclic complexes and their biological activity. Lanthanum complexes were synthesized by reacting malonodihydrazide with lanthanum perchlorate hexahydrate in the presence of various aldehydes. The complexes were characterized using elemental analysis, infrared spectroscopy, UV-visible spectroscopy, magnetic moment measurements, and thermal analysis. The complexes exhibited antibacterial activity against several pathogenic bacteria.
The document reports on the synthesis, characterization, and antimicrobial activities of metal(II) complexes of glycine and phenylalanine amino acids. Metal(II) ions (Mn, Co, Ni, Cu, Cd) reacted with the ligands (L1 = glycine, L2 = phenylalanine) in a 1:3 metal-to-ligand ratio to form coordination complexes. Spectroscopic data indicated the ligands coordinated through their amino and carboxylate groups, with the copper complexes adopting a dinuclear square pyramidal geometry and the other complexes hexacoordinate octahedral geometry. The complexes demonstrated better antimicrobial activity than acriflavine against various microbes like bacteria and fungi
56.Synthesis, Characterization and Antibacterial activity of iron oxide Nanop...Annadurai B
This document summarizes the synthesis, characterization, and antibacterial activity of iron oxide nanoparticles. Key points:
- Iron oxide nanoparticles were synthesized using a co-precipitation method by adding mixtures of metal salts to a sodium hydroxide solution, producing particles between 14-68 nm in size.
- Characterization using XRD, FTIR, VSM, and SEM confirmed the crystalline cubic spinel structure and magnetic properties of the nanoparticles. Particle size decreased with increased manganese substitution.
- Magnetic measurements showed saturation magnetization and coercivity decreased with increased manganese content due to changes in exchange interactions between metal sites.
- Antibacterial tests showed the nanoparticles had moderate antibacterial effects against E
The Influence of a New-Synthesized Complex Compounds of Ni (II), Cu (II) And ...IOSR Journals
This document describes the synthesis and characterization of new macrocyclic complex compounds containing nickel(II), copper(II), and iron(II) coordinated with a ligand containing a tetraoxotetrahydrazin moiety. The complexes were characterized using techniques such as elemental analysis, UV-visible and IR spectroscopy, and magnetic moment measurements. The complexes were then tested for antibacterial activity against 14 pathogenic bacteria and compared to a standard antibiotic. The results indicate that the new complexes show potential as antimicrobial agents.
This document describes the synthesis and characterization of new macrocyclic complex compounds containing nickel(II), copper(II), and iron(II) coordinated with a ligand containing a tetraoxotetrahydrazin moiety. The complexes were characterized using techniques such as elemental analysis, UV-visible and IR spectroscopy, and magnetic moment measurements. The complexes were then tested for antibacterial activity against 14 pathogenic bacteria and compared to a standard antibiotic. The results indicate that the new complexes show potential as antimicrobial agents.
International Journal of Engineering and Science Invention (IJESI)inventionjournals
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
Synthesis and Characterization of Thermal Analysis of La (Ii) Macrocyclic Com...inventionjournals
The macrocyclic complex compounds of La(II) containing a ligand having tetraoxotetrahydrazin moity are synthesized by template condensation of malonodihydrazide (C3H8N4O2) with different aldehydes. The complexes are characterized on the basis of elemental analysis, UV-visible & IR spectroscopy, magnetic moment and conductance measurement and other physical properties.Antibacterial activity of the derived complex compounds, as well as already used standard compound kanamycin, was tested on fourteen pathogenic bacteria. Given results were then compared to the efficacy of the Antibacterial activity of standard compound kanamycin used for control of these pathogenic bacteria.
SYNTHESIS AND CHARACTERIZATION OF THERMAL ANALYSIS OF La (II) MACROCYCLIC COM...inventionjournals
This document summarizes the synthesis and characterization of lanthanum (II) macrocyclic complexes and their biological activity. Lanthanum complexes were synthesized by reacting malonodihydrazide with lanthanum perchlorate hexahydrate in the presence of various aldehydes. The complexes were characterized using elemental analysis, infrared spectroscopy, UV-visible spectroscopy, magnetic moment measurements, and thermal analysis. The complexes exhibited antibacterial activity against several pathogenic bacteria.
The document reports on the synthesis, characterization, and antimicrobial activities of metal(II) complexes of glycine and phenylalanine amino acids. Metal(II) ions (Mn, Co, Ni, Cu, Cd) reacted with the ligands (L1 = glycine, L2 = phenylalanine) in a 1:3 metal-to-ligand ratio to form coordination complexes. Spectroscopic data indicated the ligands coordinated through their amino and carboxylate groups, with the copper complexes adopting a dinuclear square pyramidal geometry and the other complexes hexacoordinate octahedral geometry. The complexes demonstrated better antimicrobial activity than acriflavine against various microbes like bacteria and fungi
56.Synthesis, Characterization and Antibacterial activity of iron oxide Nanop...Annadurai B
This document summarizes the synthesis, characterization, and antibacterial activity of iron oxide nanoparticles. Key points:
- Iron oxide nanoparticles were synthesized using a co-precipitation method by adding mixtures of metal salts to a sodium hydroxide solution, producing particles between 14-68 nm in size.
- Characterization using XRD, FTIR, VSM, and SEM confirmed the crystalline cubic spinel structure and magnetic properties of the nanoparticles. Particle size decreased with increased manganese substitution.
- Magnetic measurements showed saturation magnetization and coercivity decreased with increased manganese content due to changes in exchange interactions between metal sites.
- Antibacterial tests showed the nanoparticles had moderate antibacterial effects against E
The Influence of a New-Synthesized Complex Compounds of Ni (II), Cu (II) And ...IOSR Journals
This document describes the synthesis and characterization of new macrocyclic complex compounds containing nickel(II), copper(II), and iron(II) coordinated with a ligand containing a tetraoxotetrahydrazin moiety. The complexes were characterized using techniques such as elemental analysis, UV-visible and IR spectroscopy, and magnetic moment measurements. The complexes were then tested for antibacterial activity against 14 pathogenic bacteria and compared to a standard antibiotic. The results indicate that the new complexes show potential as antimicrobial agents.
This document describes the synthesis and characterization of new macrocyclic complex compounds containing nickel(II), copper(II), and iron(II) coordinated with a ligand containing a tetraoxotetrahydrazin moiety. The complexes were characterized using techniques such as elemental analysis, UV-visible and IR spectroscopy, and magnetic moment measurements. The complexes were then tested for antibacterial activity against 14 pathogenic bacteria and compared to a standard antibiotic. The results indicate that the new complexes show potential as antimicrobial agents.
Synthesis, Characterization and antimicrobial activity of some novel sulfacet...iosrjce
IOSR Journal of Applied Chemistry (IOSR-JAC) is a double blind peer reviewed International Journal that provides rapid publication (within a month) of articles in all areas of applied chemistry and its applications. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Chemical Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
A STUDY TO EVALUATE THE IN VITRO ANTIMICROBIAL ACTIVITY AND ANTIANDROGENIC E...Dr. Pradeep mitharwal
The present paper deals with synthesis and characterization
of some new chromium (III) Schiff base complexes using microwave irradiation
technique as well as conventional heating. The S∩N donor benzothiazolines, 1-
(2-furanyl) ethanone benzothiazoline (Bzt1N
∩
SH), 1-(2-thienyl) ethanone
benzothiazoline (Bzt2N
∩
SH) and 1-(2-pyridyl) ethanone benzothiazoline
(Bzt3N
∩
SH) were prepared by the condensation of ortho-aminothiophenol with
respective ketones in ethanol.
This document summarizes the synthesis and characterization of mixed ligand complexes of a symmetrical Schiff base ligand and nicotinamide with various metal ions. A new symmetrical Schiff base ligand was prepared via the condensation of hydrazine hydrate and 4-hydroxy-3-methoxybenzaldehyde. Mixed ligand complexes were synthesized using a 1:1:2 molar ratio of metal salt, Schiff base ligand, and nicotinamide. The complexes were characterized using various techniques such as elemental analysis, conductivity measurements, IR and UV-Vis spectroscopy, and magnetic susceptibility measurements. The ligand and complexes were also tested for their antimicrobial activity against various bacteria. In general, the complexes showed enhanced antibacterial activity compared to the free ligands
This document describes the synthesis, spectral characterization, and biological screening of transition metal complexes of the ligand 2-(5-mercapto-1,3,4-oxadiazol-2-yl)phenol. A series of complexes were prepared using Cu(II), Co(II), Ni(II), and Zn(II) and characterized using analytical data, magnetic susceptibility, IR, UV-Vis, 1H NMR, 13C NMR, EPR, and other techniques. Spectral data suggest an octahedral geometry around the metal ion. Biological screening showed the complexes have antibacterial, antifungal, and DNA cleavage activities.
This document reports on the synthesis and characterization of polyethyleneimine-anchored copper(II) complexes and their in vitro DNA binding studies and cytotoxicity. Specifically, it synthesized copper(II) complexes containing 1,10-phenanthroline and L-tyrosine ligands bound to a branched polyethyleneimine polymer. It characterized the complexes using various techniques and studied their binding to calf thymus DNA. It found that the complex with the highest degree of copper(II) coordination bound most strongly to DNA. Finally, it evaluated the cytotoxic activity of this complex against MCF-7 breast cancer cells.
This document presents a layout for a presentation on synthesizing and characterizing iron oxide nanoparticles. The presentation aims to develop an alternative green method for synthesizing iron oxide nanoparticles from locally available tea leaves and to investigate their antibacterial and antifungal properties. The experimental section describes synthesizing iron oxide nanoparticles from tea leaf extract and coating them with chitosan. Characterization techniques like SEM, XRD, and FTIR are used to analyze the nanoparticles. Antibacterial tests on E. coli and antifungal tests on Candida albicans show the coated nanoparticles have antibacterial and antifungal properties. The expected outcome is that the green synthesis method could be used to develop novel biomaterials and the nanoparticles could help treat
This study synthesized and characterized Schiff base transition metal complexes of cobalt(II) and copper(II) acetylacetonate (acac) ligands. The cobalt(II) and copper(II) acac complexes were tested for their antimicrobial properties against bacteria and fungi. Both complexes showed little to no inhibitory effects on the microbes tested. Their structures were characterized through UV-Vis spectroscopy, which identified maximum absorbances of 491 nm for cobalt(II) acac and 632 nm for copper(II) acac.
Organomercury compounds have a variety of applications despite their toxicity. This document discusses two recent research topics on the use of organomercury catalysts:
1) The development of organomercury haptens for enzyme-linked immunoassays to detect inorganic and organic mercury. Antibodies were successfully generated that could bind both mercury ions and organometallic forms of mercury.
2) A direct method for derivatizing disulfide bonds in proteins using organic mercury in alkaline medium without chemical pre-reducing agents. p-Hydroxymercurybenzoate was shown to effectively label disulfide groups in lysozyme, allowing for their one-step determination.
Overall, the document
METALLO - BIOACTIVE COMPOUNDS AS POTENTIAL NOVEL ANTICANCER THERAPYijac123
Mono and bi-organometallic complexes of Cu(II), Ni(II), Mn(II), Zn(II) and Ag(I) complexes with
oxaloamide ligand has much potential as therapeutic and diagnostic agents. The ligand allows the
thermodynamic and kinetic reactivity of the metal ion to be controlled and also provide a scaffold for
functionalization. Specific examples involving the design of metal complexes as anticancer agents are
discussed. These complexes have been synthesized and characterized by (1H-NMR, mass, IR, UV-VIS,
ESR) spectra, magnetic moments and conductance measurements, elemental and thermal analyses. Molar
conductances in DMF solution indicates that, the complexes are non-electrolytes. The ESR spectra of solid
Cu(II) complexes (2-5) show an axial type indicating a d(X2-y2) ground state with a significant covalent
bond character. However, Mn(II) complex(9), shows an isotropic type indicating an octahedral geometry.
Cytotoxic evolution IC50 of the ligand and its complexes have been carried out. Cu(II) Complexes show
enhanced activity in comparison to the parent ligand or standard drug. Copper is enriched in various
human cancer tissues and is a co-factor essential for tumor angiogenesis processes. However, the use of
copper binding ligand to target tumor, copper could provide a novel strategy for cancer selective
treatment.
This document summarizes a study on the inhibition of human alkaline phosphatases by vanadate. The key findings are:
1) Vanadate (orthovanadate) was found to be a potent competitive inhibitor of purified alkaline phosphatase from human liver, intestine and kidney, with a Ki of less than 1 microM.
2) The inhibitory effect of vanadate was reversed and full enzymatic activity was restored in the presence of 1mM adrenaline.
3) Phosphate and vanadate were found to compete for the same binding site on the enzyme.
Synthesis, structural characterization and biological activity of Cu(II), Co(...IJAEMSJORNAL
A novel series of metal complexes of 2-(thiazol-2-ylimino) thiazolidin-4-one ligand were prepared; the corresponding ligand was synthesized from reaction 2-Chloro-N-(thiazol-2-yl) acetamide with ammonium thiocyanate. The complexes are characterized by FTIR, UV-Vis, molar conductance and mass spectroscopy. The low molar conductance values indicate that the complexes are non-electrolytes.Spectroscopic studies confirmed that the ligand bonded to the metals through the sulphur atoms. Coordination number of copper and nickel complexes is four with square planar geometry, while the cobalt complex has octahedral geometry.In vitro antibacterial activity of ligand and its metal complexes was evaluated using well diffusion method and compared to the standard drug (tetracycline). The antibacterial activitywas examined against Escherichia coli, and pseudomonas aeruginosa, as gram negative bacteria and Staphylococcus aureus as gram positive bacteria. It was found that Nickel complex has the highest antibacterial activity among the synthesized compounds with Zone inhibition diameter in the range 25-29 mm.
Chelation Trends and Antibacterial Activity of Some Mixed Ligand ChelatesTaghreed Al-Noor
Synthesis and investigation of new Co(II), Ni(II), Cu(II), Zn(II) and Cr(III)chelates of mixed ligands including
aSchiff base [(E)-2-(4-(dimethylamino)benzylideneamino)phenol] (C15H16N2O) derived from the condensation of 4-
dimethylaminobenzaldehyde with 2-aminophenol as main ligand (L1) and an amino acid; L-Histidine as co-ligand (L2)
were studied. The obtained Schiff base and the mixed ligand chelates were subjected to several physiochemical
techniques, in terms of CHN elemental analyses, molar conductivity, magnetic moment measurements, infrared,
electronic and mass spectroscopies. The CHN analytical data showed the formation of the Schiff base compound and the
mixed ligand chelates in 1:1:1[M:L1:L2] ratio. All the prepared mixed ligand chelates were non-electrolyte in nature.
The infrared spectral data exhibited that the used ligands behaving as bidentate ligands towards the metal ions. The
1HNMR spectra of the ligands and their Zn(II) mixed ligand chelate exhibited the effect of the activated groups of the
ligands by the metal ion. The electronic spectral results showed the existence of π→π* (phenyl ring) and n→π*(HC=N)
and suggested the geometrical structures of the chelates. Meanwhile, the mass spectral data revealed the fragmentations
of the Schiff base, Histidine and their Cu(II) mixed ligand chelate. The studies made on these chelates proposed a six
coordinated octahedral geometry for all these chelates. The antibacterial activities of the Schiff base, Histidine, metal
salts and mixed ligand chelates were screened. It is found that the mixed ligand chelates have the most biological activity
in comparison to the free ligands and salts.
Keywords: Schiff base; 4-dimethylaminobenzaldehyde; 2-aminophenol; Histidine; mixed ligand chelates;
Physiochemical techniques; Antibacterial activity.
Synthesis, Characterization and Antibacterial Activity of New Complexes of So...IOSR Journals
Complexes of some lanthanide picrates (Ln3+ = Pr3+, Nd3+ and Dy3+) with benzo-18-crown-6 and 221-cryptand were synthesized and characterized by elemental analysis, FTIR, and UV-Visible. Spectrophotometric methods, thermal analysis (TGA & DTG), melting point, magnetic susceptibility and molar conductance. Also an in-vitro study on gram positive (Staphylococcus aureus) and gram negative bacteria (Escherichia coli, Salmonella and pseudomonas aeruginosa) was performed and the results were compared to those of the broad spectrum antibiotic Chloramphinicol. The benzo-18-crown-6 complexes have the general formula of [Ln.L.(Pic)2]Pic.nH2O , where; (Ln3+ = Pr3+, Nd3+, and Dy3+) , (L = Benzo-18-crown-6) , (Pic = Picrate anion) , (n = 1-2). In these complexes two picrate anions are coordinated to the metal ion through the phenolic oxygen and oxygen of the ortho nitro group, thus, the metal ions in these complexes have a coordination number of (10). The complexes of 221-cryptand have the general formula of [Ln.L.(Pic)]Pic2.nH2O where; (Ln3+ = Pr3+, Nd3+, and Dy3+), (L = 221-cryptand), (Pic = Picrate anion), (n = 1,2 or 7). In these complexes one picrate anion is coordinated to the metal ion, also through the phenolic oxygen and the oxygen from the ortho nitro group, thus the metal ions in the cryptand complexes have a coordination number of (9).
ZnO nanoparticles were synthesized using a combustion method with low-temperature solution combustion. XRD and SEM characterization confirmed the formation of hexagonal wurtzite ZnO nanoparticles around 30-40nm in size. The antibacterial activity of the ZnO nanoparticles was tested against E. coli using colony counting and disk diffusion methods. Both methods showed the ZnO nanoparticles had antibacterial effects in a concentration-dependent manner, with 100μg/L ZnO demonstrating the strongest antibacterial activity through over 70% bacterial reduction and the largest inhibition zone of 24mm. The ZnO nanoparticles were also found to damage the genomic DNA of treated E. coli cells.
Determination of Stability Constants and Gibbs Free Energies of Cefotaxime Zn...ijtsrd
Cefotaxime is a synthetic lactam antibiotic that is active against Gram negative and Gram positive bacteria. Cefotaxime is able to chelate metal ions due to the presence of C=O, NH2, COOH, COOR, NH and NO electron donating groups. The stability constants and Gibbs free energies of cefotaxime Zn II were determined colorimetrically at 25 and 40 oC using continuous variation and mole ratio methods. The formation of Zn II complex with cefotaxime was studied colorimetrically at an absorption maximum of 430 nm at different temperatures. The data showed that Zn II and cefotaxime combine in the molar ratio of 1 2 at pH 7.4 with ionic strength maintained using 0.1M KNO3. Calculated stability constants values were 1.96 x 105 and 1.28 x 105 using continuous variation method and 1.11 x 105 and 1.11 x 105 using mole ratio methods at 25 and 40 oC respectively. Calculated GO for the complex were 3.01 x 104 and 3.06 x 104 J using continuous variation method and 2.88 x 104 J and 3.02 x 104 J using mole ratio method at 25 and 40 oC respectively. The stability constant results suggested that cefotaxime used in the study is a good chelating agent and can be an efficient antidote in the therapy of Zn II overload or poisoning. O. V. Ikpeazu | I. E. Otuokere | K. K. Igwe "Determination of Stability Constants and Gibbs Free Energies of Cefotaxime-Zn(II) Complex at Different Temperatures" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-4 | Issue-5 , August 2020, URL: https://www.ijtsrd.com/papers/ijtsrd31797.pdf Paper Url :https://www.ijtsrd.com/chemistry/other/31797/determination-of-stability-constants-and-gibbs-free-energies-of-cefotaximeznii-complex-at-different-temperatures/o-v-ikpeazu
This thesis examines the use of quantum mechanical modeling to understand organic compound sorption reactions with iron oxides. The student used computational modeling software to calculate the relative Gibbs free energy of selected organic acids sorbing to iron oxides. Theoretical spectra generated from the modeling were evaluated against previous experimental IR spectra to validate the modeling approach. Overall, the research aims to demonstrate that advanced quantum mechanical modeling is an effective technique for predicting sorption mechanisms and understanding organic contaminant behavior in the environment.
The document summarizes research on the biological synthesis of silver nanoparticles using Klebsiella pneumonia bacteria. Silver nanoparticles were successfully synthesized using the cell-free supernatant of K. pneumonia when added to silver nitrate solutions. The nanoparticles were characterized using UV-VIS spectroscopy, SEM, and FTIR, and were found to be spherical in shape with sizes around 21nm. Antimicrobial testing showed the biologically synthesized silver nanoparticles were effective against both gram-positive and gram-negative bacteria. Potential applications of the silver nanoparticles include use in wound dressings and antimicrobial fabrics.
International Journal of Engineering and Science Invention (IJESI)inventionjournals
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
This study synthesized a Schiff base ligand (N, N’ (2 hydroxybenzaldehyde) diamino diphenyl ether [HL]) and its Co(II) and Cu(II) metal complexes. The ligand and complexes were characterized using techniques like UV-visible, FTIR, and 1H NMR spectroscopy. The ligand and complexes were also screened for their antimicrobial activity against Staphylococcus aureus and Pseudomonas aeruginosa bacteria. The Co and Cu complexes showed octahedral geometry and moderate activity against S. aureus, with the Cu complex exhibiting the highest activity.
This document reports on the synthesis and characterization of a Schiff base ligand and its cobalt and copper metal complexes. The ligand N,N’-(2-hydroxybenzaldehyde)diamino diphenyl ether was synthesized by condensing 2-hydroxybenzaldehyde and 4,4’-diaminodiphenyl ether. Cobalt and copper complexes were prepared by reacting the ligand with cobalt chloride and copper chloride respectively. The ligand and complexes were characterized using techniques such as UV-visible, FTIR, and NMR spectroscopy. They exhibited octahedral geometry. The ligand and complexes were also screened for antimicrobial activity, with the copper complex showing the highest activity against Staphylococcus aureus.
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Synthesis, Characterization and antimicrobial activity of some novel sulfacet...iosrjce
IOSR Journal of Applied Chemistry (IOSR-JAC) is a double blind peer reviewed International Journal that provides rapid publication (within a month) of articles in all areas of applied chemistry and its applications. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Chemical Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
A STUDY TO EVALUATE THE IN VITRO ANTIMICROBIAL ACTIVITY AND ANTIANDROGENIC E...Dr. Pradeep mitharwal
The present paper deals with synthesis and characterization
of some new chromium (III) Schiff base complexes using microwave irradiation
technique as well as conventional heating. The S∩N donor benzothiazolines, 1-
(2-furanyl) ethanone benzothiazoline (Bzt1N
∩
SH), 1-(2-thienyl) ethanone
benzothiazoline (Bzt2N
∩
SH) and 1-(2-pyridyl) ethanone benzothiazoline
(Bzt3N
∩
SH) were prepared by the condensation of ortho-aminothiophenol with
respective ketones in ethanol.
This document summarizes the synthesis and characterization of mixed ligand complexes of a symmetrical Schiff base ligand and nicotinamide with various metal ions. A new symmetrical Schiff base ligand was prepared via the condensation of hydrazine hydrate and 4-hydroxy-3-methoxybenzaldehyde. Mixed ligand complexes were synthesized using a 1:1:2 molar ratio of metal salt, Schiff base ligand, and nicotinamide. The complexes were characterized using various techniques such as elemental analysis, conductivity measurements, IR and UV-Vis spectroscopy, and magnetic susceptibility measurements. The ligand and complexes were also tested for their antimicrobial activity against various bacteria. In general, the complexes showed enhanced antibacterial activity compared to the free ligands
This document describes the synthesis, spectral characterization, and biological screening of transition metal complexes of the ligand 2-(5-mercapto-1,3,4-oxadiazol-2-yl)phenol. A series of complexes were prepared using Cu(II), Co(II), Ni(II), and Zn(II) and characterized using analytical data, magnetic susceptibility, IR, UV-Vis, 1H NMR, 13C NMR, EPR, and other techniques. Spectral data suggest an octahedral geometry around the metal ion. Biological screening showed the complexes have antibacterial, antifungal, and DNA cleavage activities.
This document reports on the synthesis and characterization of polyethyleneimine-anchored copper(II) complexes and their in vitro DNA binding studies and cytotoxicity. Specifically, it synthesized copper(II) complexes containing 1,10-phenanthroline and L-tyrosine ligands bound to a branched polyethyleneimine polymer. It characterized the complexes using various techniques and studied their binding to calf thymus DNA. It found that the complex with the highest degree of copper(II) coordination bound most strongly to DNA. Finally, it evaluated the cytotoxic activity of this complex against MCF-7 breast cancer cells.
This document presents a layout for a presentation on synthesizing and characterizing iron oxide nanoparticles. The presentation aims to develop an alternative green method for synthesizing iron oxide nanoparticles from locally available tea leaves and to investigate their antibacterial and antifungal properties. The experimental section describes synthesizing iron oxide nanoparticles from tea leaf extract and coating them with chitosan. Characterization techniques like SEM, XRD, and FTIR are used to analyze the nanoparticles. Antibacterial tests on E. coli and antifungal tests on Candida albicans show the coated nanoparticles have antibacterial and antifungal properties. The expected outcome is that the green synthesis method could be used to develop novel biomaterials and the nanoparticles could help treat
This study synthesized and characterized Schiff base transition metal complexes of cobalt(II) and copper(II) acetylacetonate (acac) ligands. The cobalt(II) and copper(II) acac complexes were tested for their antimicrobial properties against bacteria and fungi. Both complexes showed little to no inhibitory effects on the microbes tested. Their structures were characterized through UV-Vis spectroscopy, which identified maximum absorbances of 491 nm for cobalt(II) acac and 632 nm for copper(II) acac.
Organomercury compounds have a variety of applications despite their toxicity. This document discusses two recent research topics on the use of organomercury catalysts:
1) The development of organomercury haptens for enzyme-linked immunoassays to detect inorganic and organic mercury. Antibodies were successfully generated that could bind both mercury ions and organometallic forms of mercury.
2) A direct method for derivatizing disulfide bonds in proteins using organic mercury in alkaline medium without chemical pre-reducing agents. p-Hydroxymercurybenzoate was shown to effectively label disulfide groups in lysozyme, allowing for their one-step determination.
Overall, the document
METALLO - BIOACTIVE COMPOUNDS AS POTENTIAL NOVEL ANTICANCER THERAPYijac123
Mono and bi-organometallic complexes of Cu(II), Ni(II), Mn(II), Zn(II) and Ag(I) complexes with
oxaloamide ligand has much potential as therapeutic and diagnostic agents. The ligand allows the
thermodynamic and kinetic reactivity of the metal ion to be controlled and also provide a scaffold for
functionalization. Specific examples involving the design of metal complexes as anticancer agents are
discussed. These complexes have been synthesized and characterized by (1H-NMR, mass, IR, UV-VIS,
ESR) spectra, magnetic moments and conductance measurements, elemental and thermal analyses. Molar
conductances in DMF solution indicates that, the complexes are non-electrolytes. The ESR spectra of solid
Cu(II) complexes (2-5) show an axial type indicating a d(X2-y2) ground state with a significant covalent
bond character. However, Mn(II) complex(9), shows an isotropic type indicating an octahedral geometry.
Cytotoxic evolution IC50 of the ligand and its complexes have been carried out. Cu(II) Complexes show
enhanced activity in comparison to the parent ligand or standard drug. Copper is enriched in various
human cancer tissues and is a co-factor essential for tumor angiogenesis processes. However, the use of
copper binding ligand to target tumor, copper could provide a novel strategy for cancer selective
treatment.
This document summarizes a study on the inhibition of human alkaline phosphatases by vanadate. The key findings are:
1) Vanadate (orthovanadate) was found to be a potent competitive inhibitor of purified alkaline phosphatase from human liver, intestine and kidney, with a Ki of less than 1 microM.
2) The inhibitory effect of vanadate was reversed and full enzymatic activity was restored in the presence of 1mM adrenaline.
3) Phosphate and vanadate were found to compete for the same binding site on the enzyme.
Synthesis, structural characterization and biological activity of Cu(II), Co(...IJAEMSJORNAL
A novel series of metal complexes of 2-(thiazol-2-ylimino) thiazolidin-4-one ligand were prepared; the corresponding ligand was synthesized from reaction 2-Chloro-N-(thiazol-2-yl) acetamide with ammonium thiocyanate. The complexes are characterized by FTIR, UV-Vis, molar conductance and mass spectroscopy. The low molar conductance values indicate that the complexes are non-electrolytes.Spectroscopic studies confirmed that the ligand bonded to the metals through the sulphur atoms. Coordination number of copper and nickel complexes is four with square planar geometry, while the cobalt complex has octahedral geometry.In vitro antibacterial activity of ligand and its metal complexes was evaluated using well diffusion method and compared to the standard drug (tetracycline). The antibacterial activitywas examined against Escherichia coli, and pseudomonas aeruginosa, as gram negative bacteria and Staphylococcus aureus as gram positive bacteria. It was found that Nickel complex has the highest antibacterial activity among the synthesized compounds with Zone inhibition diameter in the range 25-29 mm.
Chelation Trends and Antibacterial Activity of Some Mixed Ligand ChelatesTaghreed Al-Noor
Synthesis and investigation of new Co(II), Ni(II), Cu(II), Zn(II) and Cr(III)chelates of mixed ligands including
aSchiff base [(E)-2-(4-(dimethylamino)benzylideneamino)phenol] (C15H16N2O) derived from the condensation of 4-
dimethylaminobenzaldehyde with 2-aminophenol as main ligand (L1) and an amino acid; L-Histidine as co-ligand (L2)
were studied. The obtained Schiff base and the mixed ligand chelates were subjected to several physiochemical
techniques, in terms of CHN elemental analyses, molar conductivity, magnetic moment measurements, infrared,
electronic and mass spectroscopies. The CHN analytical data showed the formation of the Schiff base compound and the
mixed ligand chelates in 1:1:1[M:L1:L2] ratio. All the prepared mixed ligand chelates were non-electrolyte in nature.
The infrared spectral data exhibited that the used ligands behaving as bidentate ligands towards the metal ions. The
1HNMR spectra of the ligands and their Zn(II) mixed ligand chelate exhibited the effect of the activated groups of the
ligands by the metal ion. The electronic spectral results showed the existence of π→π* (phenyl ring) and n→π*(HC=N)
and suggested the geometrical structures of the chelates. Meanwhile, the mass spectral data revealed the fragmentations
of the Schiff base, Histidine and their Cu(II) mixed ligand chelate. The studies made on these chelates proposed a six
coordinated octahedral geometry for all these chelates. The antibacterial activities of the Schiff base, Histidine, metal
salts and mixed ligand chelates were screened. It is found that the mixed ligand chelates have the most biological activity
in comparison to the free ligands and salts.
Keywords: Schiff base; 4-dimethylaminobenzaldehyde; 2-aminophenol; Histidine; mixed ligand chelates;
Physiochemical techniques; Antibacterial activity.
Synthesis, Characterization and Antibacterial Activity of New Complexes of So...IOSR Journals
Complexes of some lanthanide picrates (Ln3+ = Pr3+, Nd3+ and Dy3+) with benzo-18-crown-6 and 221-cryptand were synthesized and characterized by elemental analysis, FTIR, and UV-Visible. Spectrophotometric methods, thermal analysis (TGA & DTG), melting point, magnetic susceptibility and molar conductance. Also an in-vitro study on gram positive (Staphylococcus aureus) and gram negative bacteria (Escherichia coli, Salmonella and pseudomonas aeruginosa) was performed and the results were compared to those of the broad spectrum antibiotic Chloramphinicol. The benzo-18-crown-6 complexes have the general formula of [Ln.L.(Pic)2]Pic.nH2O , where; (Ln3+ = Pr3+, Nd3+, and Dy3+) , (L = Benzo-18-crown-6) , (Pic = Picrate anion) , (n = 1-2). In these complexes two picrate anions are coordinated to the metal ion through the phenolic oxygen and oxygen of the ortho nitro group, thus, the metal ions in these complexes have a coordination number of (10). The complexes of 221-cryptand have the general formula of [Ln.L.(Pic)]Pic2.nH2O where; (Ln3+ = Pr3+, Nd3+, and Dy3+), (L = 221-cryptand), (Pic = Picrate anion), (n = 1,2 or 7). In these complexes one picrate anion is coordinated to the metal ion, also through the phenolic oxygen and the oxygen from the ortho nitro group, thus the metal ions in the cryptand complexes have a coordination number of (9).
ZnO nanoparticles were synthesized using a combustion method with low-temperature solution combustion. XRD and SEM characterization confirmed the formation of hexagonal wurtzite ZnO nanoparticles around 30-40nm in size. The antibacterial activity of the ZnO nanoparticles was tested against E. coli using colony counting and disk diffusion methods. Both methods showed the ZnO nanoparticles had antibacterial effects in a concentration-dependent manner, with 100μg/L ZnO demonstrating the strongest antibacterial activity through over 70% bacterial reduction and the largest inhibition zone of 24mm. The ZnO nanoparticles were also found to damage the genomic DNA of treated E. coli cells.
Determination of Stability Constants and Gibbs Free Energies of Cefotaxime Zn...ijtsrd
Cefotaxime is a synthetic lactam antibiotic that is active against Gram negative and Gram positive bacteria. Cefotaxime is able to chelate metal ions due to the presence of C=O, NH2, COOH, COOR, NH and NO electron donating groups. The stability constants and Gibbs free energies of cefotaxime Zn II were determined colorimetrically at 25 and 40 oC using continuous variation and mole ratio methods. The formation of Zn II complex with cefotaxime was studied colorimetrically at an absorption maximum of 430 nm at different temperatures. The data showed that Zn II and cefotaxime combine in the molar ratio of 1 2 at pH 7.4 with ionic strength maintained using 0.1M KNO3. Calculated stability constants values were 1.96 x 105 and 1.28 x 105 using continuous variation method and 1.11 x 105 and 1.11 x 105 using mole ratio methods at 25 and 40 oC respectively. Calculated GO for the complex were 3.01 x 104 and 3.06 x 104 J using continuous variation method and 2.88 x 104 J and 3.02 x 104 J using mole ratio method at 25 and 40 oC respectively. The stability constant results suggested that cefotaxime used in the study is a good chelating agent and can be an efficient antidote in the therapy of Zn II overload or poisoning. O. V. Ikpeazu | I. E. Otuokere | K. K. Igwe "Determination of Stability Constants and Gibbs Free Energies of Cefotaxime-Zn(II) Complex at Different Temperatures" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-4 | Issue-5 , August 2020, URL: https://www.ijtsrd.com/papers/ijtsrd31797.pdf Paper Url :https://www.ijtsrd.com/chemistry/other/31797/determination-of-stability-constants-and-gibbs-free-energies-of-cefotaximeznii-complex-at-different-temperatures/o-v-ikpeazu
This thesis examines the use of quantum mechanical modeling to understand organic compound sorption reactions with iron oxides. The student used computational modeling software to calculate the relative Gibbs free energy of selected organic acids sorbing to iron oxides. Theoretical spectra generated from the modeling were evaluated against previous experimental IR spectra to validate the modeling approach. Overall, the research aims to demonstrate that advanced quantum mechanical modeling is an effective technique for predicting sorption mechanisms and understanding organic contaminant behavior in the environment.
The document summarizes research on the biological synthesis of silver nanoparticles using Klebsiella pneumonia bacteria. Silver nanoparticles were successfully synthesized using the cell-free supernatant of K. pneumonia when added to silver nitrate solutions. The nanoparticles were characterized using UV-VIS spectroscopy, SEM, and FTIR, and were found to be spherical in shape with sizes around 21nm. Antimicrobial testing showed the biologically synthesized silver nanoparticles were effective against both gram-positive and gram-negative bacteria. Potential applications of the silver nanoparticles include use in wound dressings and antimicrobial fabrics.
International Journal of Engineering and Science Invention (IJESI)inventionjournals
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
This study synthesized a Schiff base ligand (N, N’ (2 hydroxybenzaldehyde) diamino diphenyl ether [HL]) and its Co(II) and Cu(II) metal complexes. The ligand and complexes were characterized using techniques like UV-visible, FTIR, and 1H NMR spectroscopy. The ligand and complexes were also screened for their antimicrobial activity against Staphylococcus aureus and Pseudomonas aeruginosa bacteria. The Co and Cu complexes showed octahedral geometry and moderate activity against S. aureus, with the Cu complex exhibiting the highest activity.
This document reports on the synthesis and characterization of a Schiff base ligand and its cobalt and copper metal complexes. The ligand N,N’-(2-hydroxybenzaldehyde)diamino diphenyl ether was synthesized by condensing 2-hydroxybenzaldehyde and 4,4’-diaminodiphenyl ether. Cobalt and copper complexes were prepared by reacting the ligand with cobalt chloride and copper chloride respectively. The ligand and complexes were characterized using techniques such as UV-visible, FTIR, and NMR spectroscopy. They exhibited octahedral geometry. The ligand and complexes were also screened for antimicrobial activity, with the copper complex showing the highest activity against Staphylococcus aureus.
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2. Indo-Am.J.Pharm&Bio.Sc.,2019 ISSN: 2347-2251www.iajpb.com
Vol.17,Issuse3,July2019
Antimicrobial Evaluation of Novel Metals Complexes of
Isonicotinamido-2-hydroxy-5-methoxybenzalaldimine
Mr. R. Raghuveer1
, Raj Kumar Marikanti2
, B. Narayanamma3
Abstract
The emergence of antimicrobial-resistant bacteria has increased the need for new, more effective medications to treat illnesses.
The interaction of several agents with metal ions has been proven to increase their antibacterial activity. Polydentate ligand
complexes of metal ions have been the subject of much study because of their intriguing spectroscopic, magnetic, and
biological features. The microwave synthesis method was used to create new isoniazid-based compounds and their transition
metal complexes (cobalt (II), copper (II), nickel (II), and zinc (II). Multiple spectroscopy methods (including FT-IR, UV/visible
electronic, mass, and 13C NMR and 1H NMR spectra) were used to completely describe all of the produced compounds,
including the free ligand and their metal complexes. We also used a combination of spectroscopic data including CHN, XRFA,
and AAS to determine the exact ligand to metal ratio and shape. Candida albicans (ATCC 10231), Aspergillusniger (ATCC
16404), Escherichia coli (ATCC 25922), and Staphylococcus aureus (ATCC 29213) were used in agar-well diffusion assays to
assess the antibacterial activity of the produced ligands and their complexes in vitro.
Keywords:Antimicrobialactivity;MetalcomplexesandSchiffbase
1. Introduction
There are a number of variables, such as the rise of
multidrug-resistant microbial infections and the emergence
of new infectious illnesses, that make it difficult to
effectively manage infectious diseases. New antimicrobial
agents are needed despite the availability of a number of
chemotherapeutics and antibiotics for use in medicine.
Since many bacteria have developed resistance to existing
classes of antimicrobial medications, there is also an
immediate need for novel molecules with antimicrobial
activity, most likely through new mechanisms of action.
Many biological activities rely on metal ions, including the
catalytic activity of metalloenzymes, the control of nucleic
acid replication, and the transport of oxygen via
hemoglobin's iron-porphyrin complexes. Its role as an
oxygen transporter is linked to iron's reversible control
over oxygen molecules [1]. Since amine (or Schiff base)
compounds readily form stable complexes with the vast
majority of transition metal ions [2;3], they play an
important role in inorganic chemistry. Condensation of a
carbonyl molecule with a primary amine (aldehydes or
ketones) produces an azomethine group (-N=CHR) that is
characteristic of these compounds [4]. The unsaturated
double bond and the poor electronegativity of nitrogen in
the azomethine group (>C=N) provide for a good donor
and Schiff base forming active ligands because of the
presence of a lone pair of electrons at the nitrogen atom.
How well a ligand bonds is determined by the steric and
electronegativity properties of the atoms involved in the
coordination process. Chelates' structural characteristics
provide extra steadiness to the complexes, especially those
with a five- or six-membered ring. Therefore, an additional
component in providing stability will be the existence of a
functional group next to > C=N with a replaceable
hydrogen atom.
Associate Professor1,2
,Assistant Professor3
Dept. of Pharmacology1
,Pharmaceutics2
,Pharmaceutical Analysis3
Mother Theresa Institute of Pharmaceutical Education and Research, Kurnool, Andhra Pradesh
3. Indo-Am.J.Pharm&Bio.Sc.,2019 ISSN: 2347-2251www.iajpb.com
Vol.17,Issuse3,July2019
To slow down their decomposition or polymerization, aryl
groups should be attached to the nitrogen or the carbon of
the C=N double bond [5]. Anti-inflammatory, anti-
malarial, anti-tumor, and antibacterial properties were
among the many biological actions shown by Schiff bases
[6,7], [8,9], [10–15], and [16–19].
Some Schiff bases demonstrated enhanced activity
following coordination/chelation with some metal ions,
therefore researchers focused on complexing these
compounds to identify new ones with an enhanced
pharmacological profile. Some of these complexes may be
used in a wide variety of inorganic, organic, and medicinal
applications.
key functions in orgometallic synthesis and catalysis [20-
24], as well as industrial and analytical applications.
Isonicotinic acid hydrazide (INH) is a first-line drug for
treating Mycobacterium TB and for preventing
tuberculosis infection in people with human
immunodeficiency virus [25,26]. Numerous divalent ions
may be chelated with isonicotinic acid hydrazide [27].
Attaining and characterizing the fungicide and bactericide
properties of metal ion mixed ligand complexes with
hydrazone and isoniazid derivatives [28-30].
Researchers in the field of chemistry now have a pressing
responsibility to find ways to enhance chemical processes
that will result in less pollution of the natural world [31].
The use of microwaves to aid in the synthesis of organic
and inorganic chemicals is a relatively young but rapidly
growing topic in synthetic organic chemistry. Microwave
irradiation has been shown in experiments to accelerate the
rate of certain chemical processes and increase product
yields in comparison to traditional heating methods, hence
these findings provide the basis for this novel approach. In
a number of cases, microwave chemical synthesis [32-34]
may shorten the time it takes to complete a reaction from
hours at reflux temperature under conventional conditions
to minutes or even seconds. Therefore, the purpose of this
research was to find new antibiotics that can be utilized to
treat illnesses caused by multi-drug-resistant bacteria.
Using microwave-assisted chemical synthesis, we
produced isoniazid-based compounds and their transition
metal complexes (cobalt, copper, nickel, and zinc) and
investigated their antibacterial properties.
2. Methods
2.1 Chemistry
Allthechemicalsandsolventsusedinthesynthesisof
Schiffbaseandtheircomplexesofhighestpurityandt
heywerepurchasedfromSigma
Aldrich(UK)andFluka(UK)andusedwithout
anyfurtherpurification.
2.2 Instruments
2.3 We used a microwave closed system (Milestone
start E 2450 MHz, Italy) to synthesize chemicals
(ligand and metal complexes). Pre-coated
aluminum plates (silica gel 60778, Fluka
analytical, UK) were used for thin layer
chromatographic (TLC) examination. Both short-
wave (254 nm) and long-wave (366 nm) UV
light were able to identify TLC spots. Open
capillary tubes were used together with a melting
point instrument (Electrothermal SMP30, Stuart,
UK) to get accurate readings. Using a Varian FT-
IR spectrophotometer (Cary-Varian 660,
Australia), infrared spectra of the produced
compounds were obtained between 4,000 and
400 cm1. Using Starna quartz cuvettes of one
centimeter in diameter, a Cary spectrophotometer
(5000, UVVISNIR, Varian, Australia) was used
to record UV-visible spectra. Using
tetramethylsilane as an internal standard and a
BrukerAvance 400 MHz NMR Spectrometer
(Bruker, France), we obtained proton nuclear
magnetic resonance (1H-NMR) and carbon
nuclear magnetic resonance (13C-NMR) spectra
in dimethyl sulfoxide (DMSO-d6). The
Shimadzu QP-2010 plus was used to capture EI
mass spectra at 70eV. Using Shimadzu TGA-
50H thermal analyzers, the thermogravimetric
analysis (TGA and DTG) was determined in a
dynamic nitrogen environment (30 ml/min) at a
heating rate of 10°C per minute. All testing was
conducted at either the Microanalytical Center at
Cairo University in Giza, Egypt, or the National
Medical Research Center in Zawia, Libya.
4. Indo-Am.J.Pharm&Bio.Sc.,2019 ISSN: 2347-2251www.iajpb.com
Vol.17,Issuse3,July2019
2.4 GeneralprocedureforsynthesisofN-
isonicotinamido-2-hydroxy-5-
methoxybenzalaldimine(ligand):
As shown in Scheme 1, equimolar amounts of
both starting materials (0.5 g isoniazid and 0.55
g 2-hydroxy-5-methoxybenzaldehyde) were
weighed and triturated to form a homogeneous
mixture using clean and dry Teflonvessels
withthe addition of 3-4 drops of ethanol. The
reaction mixture was subjected tomicrowave
irradiation at350 - 600 Watt power for about 2
minutes with maximum heating of 60o
C. The
optimum reaction time wasdetermined based on
the reaction completion using TLC and the
appropriate solvent system. The reaction
mixturewas allowed to cool and the crude solid
product was collected through vacuum filtration
and washed with threevolumes of acetone, dried
over anhydrous magnesium sulphate,
evaporated and finally recrystallized from
theappropriate solvent (ethanol). The achieved
crystals were dried and their melting points
were determined.
Thechemicalpuritywasinvestigated
byTLCusingchloroform/ethanol(90:10)
asmobile phases.
O NH
N
NH2
HO
+
O H
EthanolMW.2
min,350WNOCH3
O OCH3
NH
N
OH
5. Scheme1:SynthesisofcomplexesofN-isonicotinamido-2-hydroxy-5-methoxy-benzalaldimine(ligand)
2.5 Generalprocedureforsynthesisofmetalcomplexes
Metal complexes were prepared by weighing
and triturating equimolar amounts of Schiff base
ligand and metalchloride or acetate metal salts
using clean and dry Teflon vessels. The reaction
mixture was subjected to
microwaveirradiationat600-
800Wattpowerforabout3-
5minutesusing0.5mlofdryethanolasasolventafter
milling.The optimum reaction time was
determined based on the reaction completion
using TLC and the appropriate solventsystem.
The crude product achieved after filtration under
vacuum was washed several times with hot
ethanol andfinally dried and their melting points
were determined. Metal salts used were ZnCl2,
CoCl2.6H2O, CuCl2.2H2O
andNi(CH3COO)2.4H2O.
3. Biology
3.1 Evaluationofantimicrobialactivities
The Schiff base ligands and their metal
complexes were evaluated for their in vitro
antibacterial activity
againstseveralstrainsofmicroorganisms:Staphylo
coccusAureus(ATCC29213),EscherichiaColi(A
TCC25922),Candida Albicans(ATCC 10231)
and Aspergillus Niger (ATCC 16404). Strains
were obtained from the
AmericanTypeCultureCollection(ATCC)andwer
erecognizedbasedontheAmericantypeofcellcultu
recollection(ATCC) by agar-well diffusion
method. Bacteria were inoculated into nutrient
broth (Difco), incubated for twentyfour hours
and fungi kept inoculated in malt extract broth
(Difco) for forty eight hours. In the agar-well
diffusionmethod, Malt Extract Broth (Difco)
and Mueller Hinton Agar (Oxoid) were
sterilized in a flask and cooled to 45–
50°
C,andweredistributedintotwentymillilitteraliq
uotstosterilizedpetridishesafterinjectingtenmicro
litter
cultures of bacteria which was prepared as
stated earlier and were keep to solidify. The
dilution plate method wasutilized to quantify the
microorganisms (105
bacteria ml−1
and fungi
103
-104
ml−1
) for twenty four hours [35].
Wellswere dug in the culture plates by using a
sterilized cork borer (7 mm diameter). The
synthesized compounds weredissolved in
dimethyl sulfoxide (0.2 ml) and then added to
the wells aseptically. The petri dishes were left
at 4°
C fortwo hours and then the plates were
incubated at 30°
C for bacteria (18–24 hours)
and at 25°
C for fungi (72 hours). Atthe end of
the incubation period the inhibition zones
produced on the medium were assessed as
millimeters (mm).The control samples were
only loaded with only DMSO. Blank tests
showed that the concentration of DMSO
usedhasnotanyaffectandtheantimicrobialactivity
obtainedwillbecorrelatedtothesynthesizedcompo
unds.Tetracyclineand Amphotericin B
asantimicrobial agentswereused asreferences.
4. Results
4.1 Chemistrypart
7. Figure1:1
H-NMRspectrumoftheligand
4.1.2 IRspectra
ThemainstretchingfrequenciesoftheIRspectraoftheligandanditscomplexesareshowninTable2
Ligand⁄complexes ν(C=O)
Amide
ν(C=N)
Azomethine
ν(OH)
Phenolic
ν(C‒O)
Phenolic
C14H13N3O2(HL) s1652 s1578 3380 m 1261s
[Zn(L)2].1.5H2O s1679 s1542 Disappeared* 1268s
[Co(L)2] s,1608s1679
s1539 Disappeared* s1267
[Ni(L)H2O](ac) s1595 s1535 Disappeared* 19s12
[Cu(L)2].6H2O S,1562m1584
s1523 Disappeared* s1251
s:strong,m:medium
Table2:IRstretchingfrequenciesofvariousfunctionalgroupsofligandsanditsmetalcomplexes
*The peak in the Ligand spectra at 3380 cm-1
due to the deformation of OH group and disappeared in the
complexes.ThisindicatesdeprotonationofphenolicOH,oncoordinationwithmetal ion.
4.1.3 Electronicspectralanalysis
The electronic spectra of the free ligand showed
two strong absorption bands in the Ultraviolet-
Visible region (294-361 nm), allocated to the
transitions π→π* and n →π *. These transitions
are found only in the spectra of
thecomplexes.Buttheyareshiftedandstronglydisp
lacedinallcomplexes,verifyingcoordinationofme
talionstothe
9. Compounds Formula
weight
ElementalanalysisCHN
Found(Calcd.)%
XRF
(%)
AAS
(%)
C H N Cl M
[HL].
H2OC14H15
N3O4
289.29 55.64
(58.13)
5.07
(4.83)
14.08
(14.53)
……. …….
[Zn(L)2]C28H24N6O6Zn 605.94 55.26
(55.50)
3.96
(3.99)
13.81
(13.87)
˂LLD 9.02
(10.79)
[Co (L) 2].1.5 H2O
C28H27N6O75Co
626.48 55.53
(53.68)
4.25
(4.04)
13.88
(13.41)
˂LLD 10.19
(9.41)
[Ni(L)H2O](ac)
C16H17N3O6Ni
406.02 47.81
(47.33)
4.06
(4.22)
11.20
(10.35)
…… 13.75
(14.46)
[Cu (L)2].6H2O
C28H36N6O12Cu
712.16 47.86
(47.22)
3.48
(4.00)
11.27
(11.80)
˂LLD 7.03
(8.92)
LLD:LowerLimitofDetection=0.01ppm
Table4:Theresultsofelementalanalysis,AASandXRFoftheligandsandtheircomplexes:
4.1.5 Massspectra
ThemostimportantpeaksintheEImassspectraldataofallcomplexeswithligandarelistedinTable5.
Compounds m⁄z Fragments R.I(%)
C14H13N3O3 271
107
[M]+
[C7H7O]+
83.90
100
[Zn(C14H12N3O3)2] 608
605
[M+3]+
[M]+
2.87
0.53
[Co(C14H12N3O3)2] 601
600
[M+1]+
[M]+
51.43
81.90
[Ni(C14H12N3O3)H2O]+
346 [M]+
49.01
[Cu(C14H12N3O3)2] 605
604
[M+1]+
[M]+
86.79
66.04
Table5:Massfragmentationoftheligandanditsmetalcomplexes
4.1.6 Thermalanalysis(TGAandDTG)
Thermogravimetric analysis of the ligand and its complexes were used to obtain information about the
thermalstability of these new complexes. In addition, to make a decision whether the water molecules (if it is
available) areoutside or inside the inner sphere coordination of the central metal ion. The results of the thermal
analysis of theligandand itsmetalcomplexes aregiven inTable6.
10. Compounds
TGrange
(0
C)
DTG max
(0
C)
n*
Mass loss
Found (calcd)
Assignment
C14H13N3O3(HL) 58-141 103 1 5.79(6.22) Lossof1H2O(hydration)
[Zn(L)2] ...... ...... ....... ......
[Co(L)2].1.5H2O -22632 49,192 2 3.87(4.30) Lossof1.5H2O(hydration)
[Ni(L)H2O](ac) 180-328 275 1
4.89(4.43)
Lossof1H2O(coordinated)
[Cu(L)2].6H2O 258-118 223 1 15.96(15.16) Lossof6H2O(hydration)
n*=numberofdecompositionsteps;L=C14H12N3O3
Table6:Thermalanalysisoftheligandanditsmetalcomplexes
4.2 Biologypart
4.2.1 Evaluationofantimicrobialactivity
The antimicrobial activity studies of the ligand and its metal complexes were performed by using different fungi
andbacteriaand the resultsof theinhibitionaresummarizedinTable7.
Compounds Inhibitionzonediameter(mmpermgsample)
E.coli S.aureus A.flavus C.albicans
DMSO 0 0 0 0
Standard
Tetracycline 31 28 ---- ----
AmphotericinB ---- ---- 16 19
C14H13N3O3(HL) 12 16 0 9
[Zn(L)2] 16 18 0 9
[Co(L)2].1.5H2O 11 10 0 9
[Ni(L)H2O](ac) 0 0 0 0
[Cu(L)2].6H2O 12 12 0 0
Table7:Antimicrobialactivitydataoftheligandanditsmetalcomplexes
11. 5. Discussion
5.1 IRspectra
In general, the entire synthesized amides
demonstrate two absorption bands: one is the
the carbonyl absorption bandnear 1640 cm−1
which is known as amide-I band and two is the
strong band in the 1500 - 1600 cm−1
region
which isknown as amide-II band. The origin of
these two bands can be seen in hydrazones, in
which the carbonyl absorptionaccountable for
the amide-I band, which is probable to be
lowered [36;37] occasionally by the NH group
as instandard amides. The amide-I band in
isoniazide derivative, however, can be seen at
1700 and 1655 cm−1
[38]. In theentire
hydrazones, the absorptions such as 1540, 1520
cm−1
have been allocated to absorption of
amide-II. The NHstretching absorption in free
ligands occurs at ∼3300 and 3220 cm−1
as
described in the literature [39]. The
othersignificant band occurs at ∼1585-1600
cm−1
allocated to ν(C=N) (azomethine) mode
[35;39]. The strong bandsallocated at 1000–
1080 cm−1
and 1520–1575 cm−1
are possibly
allocated to symmetric and asymmetric ν(C=C)
+ν(C=N)ofthepyridineringandpyridineringdefor
mationsandbreathings,respectively[40;41].
The infrared spectra spectrum of the ligand
exhibits a strong band at 1652 cm-1
due to
ν(C=O) of the amide
group.Thebandofthisligandhasshiftedandwaspo
werfullydisplacedinallcomplexesconfirmingcoor
dinationthroughout the carbonyl oxygen. A
band at 1578 cm-1
is due to ν(C=N) azomethine
group which has shifted to
thelowerfrequenciesfortheentirecomplexes.This
suggeststheinvolvementoftheazomethinenitroge
nincoordination. Another important ligand band,
which allocated at about 3380 cm-1
owing to the
phenolic‒hydroxylgroup, was missing in the
complexes. This proofs the phenolic‒OH is
deprotonated and it is on coordination
withmetal. The band due to phenolic C‒O
stretching vibration is observed at 1261 cm-1
in
the free ligand. In the entirecomplexes this band
appears at higher or lower frequencies in 1268-
1219 cm-1
proving the participation of
thephenolic oxygen in the coordination with the
metal ions. As indicated in the literature the Ni
complex showsabsorption bands, one in the
1572 cm-1
and the other in 1425 cm-1
regions for
symmetric ν(COO¯ ) and
asymmetricν(COO¯)stretching[42;43].
5.2 Electronicspectralanalysis
Theelectronicspectrumofthezinc(II)complexsho
wsabroadabsorptionbandat444nmwhichmaybea
ssignedto a charge transfer transition, due to the
coordination of the ligand with metal ion [44].
The electronic spectrum ofthe cobalt (II)
complexis expectedto showthree absorption
bands due tothe electronic transitions,
namely4
T1g→4
T1g(P), 4
T1g(F)→4
A2g and
4
T1g→4
T2g, but bands due to these transitions
usually overlap to give a broadabsorption band.
The broad band allocated in the complex
approximately 461 nm is in agreement with
octahedralarrangements for Co (II) ion. The
electronic spectrum of the nickel (II) complex
shows two d-d absorption bands
at440and464nm,whilethethirdd-
dbandisnotobserved.Thesebandsareassignedto3
A2→3
T1(P)and3
A2→3
T1
5.3 Elementalanalysis,X-
rayfluorescenceanalysisandatomicabsorptions
pectroscopy
12. Elementalanalysisofthefreeligandandthecomple
xesofthemetalinadditiontotheatomicabsorptions
pectroscopy and the X-ray fluorescence analysis
and demonstrated in the results section (Table
4) and are in a goodconformitywith the
expectedvalues.
5.4 Massspectra
The mass spectrum of ligand showed the
molecular ion peak at m/z = 271 that
corresponds to its molecular
formula[C14H13N3O3]+
,withavirtualintensityof83
.90%.Thefragmentatm/z=107(R.I.=100%,basep
eak)isallocatedto the [C7H7O]+
ion. The other
peaks signify fragments of the molecular ion.
The EI mass spectral data of Zn(II),Co(II),
Ni(II) and Cu(II) complexes show an strong
molecular ion peak m/z [M]+
. The mass spectra
of severalcompounds also exhibit a important
peak matching to m/z [M+1]+
, [M+2]+
or [M-
1]+
and the enduring peaks signifythe successive
degradation of the complexes [46]. The peak
intensity provides an thought of the stability of
thefragments.
5.5 Thermalanalysis(TGAandDTG)
Thermogravimetricanalysisoftheligand
anditscomplexes demonstratedgoodconformity
withthe theoreticalformula as suggested from the
elemental analysis. TGA of ligand, shows the
initial weight loss 103°C is allocated
tothelossoflatticewatermoleculewhichisallocatedt
ooneH2Ocorrespondingto(found5.79%;calculated
6.22%).Theremainingsteps,thatoccurinsidethetem
peraturerange204-
799°Cattributedtodecompositionoftheligand,invol
vemasslossesof96.55%.TGAforCo(II)complex,de
monstrates2-
stagesofdecompositionwithintherangeof32-
226°
C,whichisattributabletothelossof1.5uncoordi
natedwatermolecules(weightloss;found/calculate
d.3.87⁄4.30%),whileTGforCu(II)complexshowson
estageofdecompositionwithintherangeof32-226̊
C,which isattributabletothelossof6-
uncoordinatedwatermolecules(weightloss;found⁄c
alculated.15.96⁄15.16%).Themolecularformulaeo
fthecomplexesCo(II)andCu(II)construedfromele
mentalanalysispointsouttheexistenceoflatticewate
r.IncaseNi(II) complex,TG shows onestageof
decompositionwithinthe range of 180-328̊ C,
which
isduetothelossofonecoordinatedwatermolecule(w
eightloss;found⁄calcd.4.89⁄)4.43.Butinthezinc(II)c
omplex,thereisnoconsiderableweightlossbelow18
0°Cproposingthenonappearance
oflatticewatermolecules.Thesucceedingsteps(280
-
800◦
C)inallcomplexesmatchtotheexclusionoftheo
rganicpartoftheligand[47;48].Thecomplexeshave
beensynthesizedbymicrowavemethodsfromreacti
onofCoCl2.6H2O,CuCl2.2H2O,ZnCl2andNi(CH3C
OO)2.4H2OwithSchiffbase(ligand)inpresenceofet
hanolassolvent.Formationofthecomplexesmayhav
eproceededper thefollowingequations.MCl2.nH2O
+2 L →[M(L)2].nH2O+2HCl+nH2OM=
Co(II),n=1.5;Zn(II),n=0and
Cu(II),n=6M(ac)2.4H2O+L→ [M(L)H2O]
(ac).nH2O+ CH3COOH+nH2OM=Ni(II),n=0
13. H3CO
OH2
Ni
O
N
N
H
N
The ligand acts as a monoanionic tridentate (O,
N and O) throughout the carbonyl oxygen,
phenolic oxygen andazomethine nitrogen.
Composition was construed from FT-
IR,elemental analyses, UV-VIS, XRF, AAS,
MS andTGA. The analytical data of the
complexes specify that the ligand forms a 1:2
(M : L) complex with Zn (II), Co (II)and Cu (II)
and 1:1 (M: L) with Ni (II) ions. The atomic
absorption and mass spectral data substantiate
themonomeric structure of the metal complexes
whereas the TGA studies substantiate the
existence of water moleculesin some complexes
and XRF data demonstrate that chloride anions
are absent outside the coordination sphere in
Zn(II),Co(II)andCucomplexes.Accordingtothein
dicatedanalyticalandspectraldata,thecommonstru
ctureformulaandstoichiometryofsynthetizedmeta
lcomplexes areillustratedinFigure2.
OCH3
O
M O
O
O
N
N
H
H3CO
O
nH2O ac
N
Figure 2: structural formula proposed for; (A)[M (L) 2].nH2O ,(M = Co (II), n=1.5; Zn (II), n=0 ; Cu (II), n=6)
and(B)[M(L)(H2O)](ac).nH2O,(M=Ni (II),n=0,ac=CH3COO¯)
5.6 Biologypart
5.6.1 Evaluationofantimicrobialactivity
Microorganismsrequirethe presence
ofanumberof
metalsthatplayessentialbiochemicalrolesascataly
sts,enzyme cofactors, activity in redox processes
and stabilizing protein structures [49-51].
Metals might build upexceeding normal
physiological concentrations and effecting the
transport systems, and might become toxic.
Theintracellular metals could cause toxic effects
through forming coordinate bonds with some
anions and this couldblock the efficient groups
of enzymes. This formed coordinate bonds with
the enzymes will be inhibiting
thetransportsystemsanddisturbing
cellularmembrane integrity[52;53].
It has been reported that, there are 5
fundamental mechanisms that suggest an
increased level of cellular resistance
tometals:(1)intra-
orextracellularsequestration(2)effluxofthetoxic
metalfromthecell,(3)enzymaticconversion,
(4) prohibiting by a permeability barrier, and (5)
N
H
N
N
14. bacteria and fungi, i.e. chelation may improve
or restrain the biochemical prospective of
bioactive organic species[57]. Such generation
or improvement in activity of the metal
complexes can be explained based on
Overtone’sconcept and chelation theory. Per
Overtone’s notion of cell permeability, the lipid
membrane that envelops the cellhelps the
passage of lipid soluble substances owing to
their liposolubility which is a vital factor that
managesantimicrobial activity[58]. On
chelation, the polarity of the metal ion is
abridged due to the overlap of the ligandorbital
and fractional sharing of the (+) charge of the
metal ion with donor groups. Additionally, it
enhances thedelocalization of pi-electrons over
the entire chelate ring and enhances the
lipophilicity of the complex. Thisincreased
lipophilicity in turn enhances and this could
help the penetration of the complexes into lipid
membranesandultimatelyblocksmetalactivebindi
ngsitesontheenzymesofthemicroorganisms[59;6
0].Moreover,coordination might escort to
considerable reduction of drug – resistance [61].
In addition another factors,
likeconductivity,dipolemomentandsolubilityeffe
ctedbytheexistenceofmetalionsandmightenhance
thebactericidal activity of the metal complexes
in comparison to the uncomplexed compounds
[62]. Low activity of thesome metal complexes,
as shown in this study, may be related to their
low lipophilicity which reduces penetration
ofthecomplexthroughthelipidmembraneandthere
forethesecomplexescannotachievetheirtargettobl
ockorinhibitthegrowthof microorganisms
[63;64].
In conclusion, we synthesized and characterized
four new complexes of n-isonicotinamido-2-
hydroxy-5-methoxybenzalaldimine with Cu(II),
Co(II), Ni(II) and Zn(II). The spectroscopic data
demonstrate that Schiff base acts
asmonoanionictridentateligand.Schiffbaseandso
meofthemetalcomplexeswereactiveagainstsome
ofrepresentative bacterial and fungal strains and
complexation enhances their activity. The
activity may be due toincrease in cell
permeability caused by increase of lipophilicity
of metal conjugates, which allows intracellular
drugaccumulation and target accessibility. It is
possible that intracellular reduction of metal
compounds leads to highercytoplasmic
concentration of metal species, which proves
lethal for bacteria and fungi. This study also
showssuperior antimicrobial activity of metal
complexes relative to their ligands. MIC values
indicate their potential forpharmacologicaluse.
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