Luminescent, sorptive and antibacterial potential of bismuth-organic framework

Metal organic frameworks are formed by the three-dimensional linkage of metal cores and organic linkers. In this work, bismuth-based metal organic framework (Bi-MOF) has been synthesized by using 5-hydroxyisophthalic acid (H2HIA) as linker via hydrothermal method. The said MOF was structurally characterized by UV/Vis, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), 1H NMR, energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA) and X-ray diffraction technique. This MOF showed highly porous structure with surface area 1096 m2/g as determined by BET analysis. A model batch adsorption experiment was performed to evaluate the efficiency of methylene blue (MB) dye removal from aqueous media. It was found that monolayer adsorption capacity calculated from the Langmuir isotherm was 0.6240 mg/g. Bi-MOF was also screened for its antibacterial and luminescent behavior. KEY WORDS: Bismuth, Metal-organic Frameworks, Luminescence, Sorption Bull. Chem. Soc. Ethiop. 2021, 35(1), 119-128. DOI: https://dx.doi.org/10.4314/bcse.v35i1.10

Investigations on structural, optical, and impedance spectroscopy studies of titanium dioxide nanoparticles

This article explains a novel synthesis for producing titanium dioxide (TiO2) nanoparticles by a sol-gel technique using titanium tetraisopropoxide as a titanium source. The synthesized nanoparticles were analyzed using many measurements like X-ray diffraction (XRD), HRTEM, absorption UV spectroscopy, FTIR, and ac impedance spectroscopy. X-ray peaks were used to calculate the crystallite size and lattice strain by Williamson–Hall method. Crystallite size calculated from x-ray diffraction using the Scherrer equation gives an approximate size and cannot be used for measurements. TiO2 nanoparticles are found to possess a tetragonal structure with a crystalline size around 12 nm. Particle size was confirmed by HRTEM images. The optical studies response for the nanoparticles showed the possible visible absorption peaks for TiO2 nanoparticles are 323 nm. Bandgap energy (Eg) of the TiO2 nanoparticle calculated from UV visible absorption spectra is discussed, and the bandgap is 3.14 eV. FTIR spectra showed vibration bands of the Ti-O network. AC Conductivity properties of TiO2 nanoparticles are studied in the frequency range 1 to 8 MHz at varying temperatures. The conductivity of the TiO2 nanoparticle is found to be constant in the low angular frequency region. Dielectric parameters were analyzed at different temperatures and frequencies. KEY WORDS: Conductivity, Dielectric, Nanoparticles, Titanium dioxide, Structural studies Bull. Chem. Soc. Ethiop. 2021, 35(1), 151-160. DOI: https://dx.doi.org/10.4314/bcse.v35i1.13

Synthesis, spectral and sol-gel behavior of mixed ligand complexes of titanium(IV) with oxygen, nitrogen and sulfur donor ligands

A new route to synthesize nano-sized Ti(IV) mixed ligand complexes have been investigated by the reaction of titanium(IV) chloride with ammonium salts of dithiophosphate and 3(2'-hydroxyphenyl)-5-(4-substituted phenyl) pyrazolines. The resultant complex is then treated with H2S gas to get sulfur bridged dimer of Ti(IV) complex, a precursor of TiS2. The morphology of the complexes was studied by employing XRD which shows that all the complexes are amorphous solid. Molecular weight measurements, elemental analysis in conjugation with spectroscopic (IR, 1H NMR, 13C NMR and 31P NMR) studies revealed the dimeric nature of the complexes in which pyrazoline and dithiophosphate are bidentate. Scanning electron microscopic image and XRD indicate that the particles are in the nano range (50 nm). Putting all the facts together, coordination number six is proposed for titanium with octahedral geometry. KEY WORDS: Titanium(IV), Dithiophosphate, Pyrazoline, Nano-sized, Sol-gel, Mixed ligand complexes Bull. Chem. Soc. Ethiop. 2021, 35(1), 61-76. DOI: https://dx.doi.org/10.4314/bcse.v35i1.5

Synthesis, characterization and antimicrobial activity of copper(II) Schiff base adducts of some p-substituted aniline Schiff bases

The synthesis, characterization and antimicrobial activity of Cu(II) complexes of some p-substituted aniline Schiff base ligands have been carried out. The Schiff bases were obtained from salicylaldehyde and o-vanillin. The Cu(II) complexes have been characterized by elemental analysis, conductivity measurement, infrared and electronic spectral data. The complexes were obtained either as metal chelates [Cu(L)2] or Schiff base adducts (CuCl2.2LH).xH2O. The metal chelates were non-electrolytes while the Schiff base adducts exhibited 1:1 or 2:1 electrolytes in methanol. The Cu(II) complexes exhibited slight antimicrobial activity against Escherichia coli ATCC® 8739™*, Staphylococcus aureus subsp. aureus ATCC® 6538™*, Bacillus subtilis subsp. spizizenii ATCC® 6633™* and Candida albicans ATCC® 2091™*. The complexes exhibited significant antifungal activity. KEY WORDS: Metal Chelates, Schiff bases, Adducts, Cu(II) complexes, Salicylaldimines Bull. Chem. Soc. Ethiop. 2021, 35(1), 33-42. DOI: https://dx.doi.org/10.4314/bcse.v35i1.3

Phytochemical studies of Melilotus officinalis

GC-MS analysis of the n-hexane extract of Melilotus officinalis seeds revealed twelve compounds with a combined area percentage of 98.33% predominantly, (9Z,12Z)-octadecadienoic acid (20.22%, 366 ppm), 14-methylpentadecanoic acid (19.52%, 353 ppm) and (9E)-octadecenoic acid (15.94%, 289 ppm). Two compounds, namely, cis-coumaric acid-2-O-β-D-glucopyranoside (cis-melilotoside, 1) and 1,2-benzopyrone (coumarin, 2), were isolated from the MeOH extract of the seeds of M. officinalis. The structures of isolated compounds were determined by spectroscopic techniques such as NMR, UV-Vis, and FTIR. The MeOH extract of M. Officinalis was also tested for its antioxidant activity using DPPH assay. The extract showed 29.87% DPPH inhibition at concentration of 100 μg/mL. KEY WORDS: Melilotus officinalis, Fatty acid methyl esters, Esterification, GC-MS, DPPH radical scavenging assay, Antioxidant activity Bull. Chem. Soc. Ethiop. 2021, 35(1), 141-150. DOI: https://dx.doi.org/10.4314/bcse.v35i1.12

SALLE combined with LD-DLLME for pesticides analysis in sugar and soil samples

In this study, a modified salting-out-assisted liquid-liquid extraction (SALLE) combined with low density dispersive liquid-liquid microextraction (LD-DLLME) has been developed for quantitative determination of multiclass pesticide residues (atrazine, diazinon, ametryn, terbutryn, chlorpyrifos, dimethametryn, 4,4'-dichlorodiphenyldichloroethylene (4,4'-DDE), 4,4'-dichlorodiphenyldichloroethane (4,4'-DDD) and 4,4'-dichloro- diphenyltrichloroethane (4,4'-DDT)) levels in sugar and soil samples coupled with gas chromatography–mass spectrometry (GC-MS) detection. The extract was enriched after combining SALLE to LD-DLLME and enrichment factor obtained ranged 30-121. Under the optimum conditions, the linearity of the method was in the range of 6.25–100 ng g-1 for atrazine, ametryn, terbutryn, dimethametryn and 4,4'-DDT, and in the range of 2.5–100 ng g-1 for diazinon, chlorpyrifos and 4,4'-DDD, and in the range of 1–100 for 4,4'-DDE with correlation coefficient of 0.992 or better. The limits of detection (LODs) ranged from 0.01–0.25 ng g-1. The precisions as %RSD, were below 10% for both matrices. The recoveries obtained from spiked sugar and soil samples at 5 and 50 ng g-1 ranged from 79 to 111%. The method was subsequently applied to real sugar and soil samples. All the pesticides investigated were not detected in the sugar sample. The soil sample was contaminated by atrazine and ametryn at concentration level of 0.3 and 0.2 ng g-1, respectively. KEY WORDS: SALLE, LD-DLLME, Extraction, Pesticide residues, Sugar, Soil Bull. Chem. Soc. Ethiop. 2021, 35(1), 1-16. DOI: https://dx.doi.org/10.4314/bcse.v35i1.1

Solid-state synthesis and physico-chemical characterization of modified smectites using natural clays from Burkina Faso

Solid-state intercalation was applied to prepare organo-smectites using cationic surfactants and natural clays containing smectite at various surfactant/smectite ratios. The surfactants enter the interlayers of smectites causing a swelling of the clays. The used clays were collected in Siétougou and Diabari villages located in the eastern part of Burkina Faso. The solid-state intercalation was successful for all four surfactants applied, n-dodecyltrimethylammonium bromide, (n-C12H25(CH3)3NBr), n-tetradecyltrimethylammonium bromide, (n-C14H29(CH3)3NBr), n-hexadecyltrimethylammonium bromide (n-C16H33(CH3)3NBr) and di-n-dodecyldimethyl­ammonium bromide ((n-C12H25)2(CH3)2NBr) at different levels of the cation exchange capacity (CEC). The synthesized organo-smectites were characterized regarding relative density, structural and textural properties. XRPD data showed a systematic increase of the basal spacing of the unit cell of the smectite up to >38 Å at 2.0-CEC loading of the surfactant. This increase indicates that the surfactants penetrated into the smectite interlayers with the surfactants being arranged parallel to the layers at low concentrations and almost perpendicular at high ones. FTIR spectra of the organo-smectites showed a decrease in the intensities of the water bands at around 1630 cm-1 and 3400 cm-1, and new specific bands close to 2920 cm-1 and 2850 cm-1 were assigned to the asymmetric and symmetric stretching of CH2 groups of the surfactants, respectively. KEY WORDS: Smectite, Organo-smectite, Surfactant, Intercalation Bull. Chem. Soc. Ethiop. 2021, 35(1), 43-59. DOI: https://dx.doi.org/10.4314/bcse.v35i1.4

Synthesis, characterization, in-vitro anti-inflammatory and antimicrobial screening of metal(II) mixed diclofenac and acetaminophen complexes

Mixed ligand complexes derived from diclofenac potassium salt (Kdc) and acetaminophen (ace) has been synthesized and proposed to have a general formula [MB] where M = Co2+, Ni2+, Cu2+ and Zn2+and B = (ace)(dc)(H2O)2 except for Mn2+ complex which exists as [Mn(ace)(dc)OH2]. The complexes were characterized by solubility, melting point, conductivity, elemental analyses, UV-Vis, FT-IR spectroscopy, X-ray powder diffraction (XRPD) study and magnetic susceptibility measurement. Electronic absorption spectra data are characteristic of octahedral structures for [MB]. The IR spectra revealed a bidentate coordination mode. In acetaminophen, the nitrogen and carbonyl-O atoms of the amide group were involved while the carboxylate oxygen atoms of potassium diclofenac were used; typical of a carboxylic acid derivative. The compounds were screened for in-vitro anti-inflammatory activity by inhibition of albumin denaturation assay and antimicrobial activity against bacteria strains: Bacillus subtilis, Bacillus anthrax, Escherichia coli, Salmonella typhi and a fungus Aspergillus niger. Some of the tested compounds showed moderate anti-inflammatory activity when compared to the standard drug diclofenac potassium salt. The in-vitro antimicrobial screening revealed an increased activity of the complexes against the bacteria isolates compared to the free ligands. KEY WORDS: Metal(II) ion, NSAIDs, Anti-inflammatory activity, Diclofenac potassium salt, XRPD, Antimicrobial activity Bull. Chem. Soc. Ethiop. 2021, 35(1), 77-86. DOI: https://dx.doi.org/10.4314/bcse.v35i1.6

Development and validation of a single HPLC method for the determination of thirteen pharmaceuticals in bulk and tablet dosage form

The aim of this study was to develop and validate a high performance liquid chromatography (HPLC) method for the determination of thirteen selected pharmaceutical compounds (metformin, amoxicillin, chloroquine, theophylline, trimethoprim, caffeine, norfloxacin, ciprofloxacin, acetylsalicylic acid, doxycycline hyclate, metronidazole, albendazole and cloxacillin) in bulk and tablet dosage form. Chromatographic separation using a Kromasil C18 column, gradient elution with aqueous formic acid (0.1%), methanol and acetonitrile, a UV absorption wavelength of 250 nm and a mobile phase flow rate of 1 mL/min over a 22 min run time was optimized for complete separation of the selected target compounds. The method was validated and results for: linearity, precision, sensitivity, accuracy, specificity, suitability and method robustness were obtained and met the ICH guidelines. Calibration curve correlation coefficients ranged from 0.9985-0.9998 and the percentage relative standard deviations for repeated analysis was below 5%, indicating acceptable method precision. The limits of detection (LODs) and quantification (LOQs) ranged from 0.020-0.27 µg/L and 0.080-0.91 µg/L, respectively. The accuracy study yielded recoveries in the ranges 86.0-102% for pure compounds and 90.9-106% for compounds in tablet dosage form. The method is robust for small or deliberate changes to the chromatographic parameters and found to be appropriate for analysis of tablets for the determination of the thirteen pharmaceuticals. KEY WORDS: Pharmaceuticals, Bulk determination, Tablet dosage, High performance liquid chromatography, Method development, ICH guidelines Bull. Chem. Soc. Ethiop. 2021, 35(1), 17-31. DOI: https://dx.doi.org/10.4314/bcse.v35i1.2

Synthesis, characterization, and photocatalytic efficiency of a new smart PdO oxide nanomaterials for using in the recycling and sustainable wastewater treatment

Nanostructured PdO materials with promising catalytic properties were successfully synthesized by the controlled thermal decomposition in air of three Pd(II) complexes containing Pd(II) ion, ofloxacin drug and amino acid. The Pd(II) complexes which were used as precursors were [Pd(OFL)(Gly)]Cl, [Pd(OFL)(Ala)]Cl, and [Pd(OFL)2]Cl2, where Gly is glycine amino acid, Ala is alanine amino acid, and OFL is ofloxacin. Structural and morphological properties of the synthesized PdO materials were obtained using FTIR, XRD, SEM, and EDX techniques. The XRD results confirm the tetragonal structure of PdO. The obtained PdO materials were tested as a catalyst for the heterogeneous degradation of H2O2 solution. The results revealed that PdO could effectively degrade H2O2. KEY WORDS: PdO, Nanoparticles, Photocatalytic efficiency, Wastewater treatment Bull. Chem. Soc. Ethiop. 2021, 35(1), 107-118. DOI: https://dx.doi.org/10.4314/bcse.v35i1.9