DEPARTMENT OF CHEMISTRTY

SYNTHESIS, CHARACTERISATION AND ANTIMICROBIAL ACTIVITIES OF SOME NOVEL IMIDAZOLE DERIVATIVES

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Abstract
Heterocyclic compounds are very widely distributed in nature and very abundant in plant andanimalproducts. They are included in many biochemical materials essential for life like nucleicacids(nucleotides), sugars and their derivatives, vitamin C and also, most members of vitaminBgroup(vitamin B6- pyridoxine). They are also found in application of diverse field such as agriculture,pharmaceutical and manufacturing industries. Researches have shown that heterocyclicnuclei givehigh chemotherapeutic values such as anti-malaria, anti-diabetics, anticancer and also act as aremedyfor the development of novel drugs. Imidazole containing moiety occupied a unique position in organic compounds. It is a five-memberednitrogenous heterocyclic moiety that has three carbons, two nitrogens, four hydrogen atoms, andtwodouble bonds having general molecular formula of C3H4N2. It is also known as 1,3-diazolebecauseof the nitrogen atoms present at the first and third positions (non–adjacent position) of thering, onenitrogen bear a hydrogen atom as the pyridine structure, and the other is called pyrrole typenitrogenand position four and five are equivalent. It formed the basis of many therapeutic natural productssuch as histamine, purine, histidine among others The research work focuses on the synthesis, characterization and antimicrobial activitiesofthederivatives of some new imidazole derivatives. Wallach synthesis was used to synthesize 1-methyl-5-chloro-imidazole which was nitrated to give 1-methyl-4-nitro-5-chloroimidazole. H2Sgas wasbubbleinto the solution 1-methyl-4-nitro-5-chloroimidazole in the presence of sodiumethoxide whichgave62% yield of 1-methyl-4-nitroimidazole-5-thiol (compound 4). Compound 4 was coupledwithbenzoylchloride and phenylethylbromide to produce compound 4B and 4A respectively. 1-methyl-4-nitroimidazole-5-thiol underwent oxidative chlorination to yield an unstable intermediateof1-methyl-4-nitroimidazole-5–sulfonyl chloride. All attempt to stabilized 1-methyl-4-nitroimidazole-5–sulfonyl chloride failed. With the sulfonyl chloride at position 5 on imidazole ring, it wasthencoupled with proline, proline methylester, biphenylhydroxide, 2-aminophenol and N- ethylanilinewhich yielded 1-methyl-4-nitroimidazole-5- lphonylproline,1-methyl-4-nitroimidazole-5-sulphonylprolinemethylester, 1-methyl-4-nitroimidazole-5-sulphonyl(2-hydroxylbiphenyl), 1-methyl-4-nitroimidazole-5-sulphonyl(2-aminophenol),1-methyl-4-nitroimidazole-5-sulphonyl(N- ethylaniline). The 4-nitro-2-methyl-1-H-ethanolyimidazole was chlorosulfonated with thionyl chloride, andthencoupled with aniline and 2,4 dichloroaniline to give 1-chloroethane-2-[thioacylaniline-4-nitroimidazole and 1-chloroethane-2-[thioacyl-(2,4-dichloroaniline)]-4-nitroimidazole respectively.The synthesized compounds were purified and confirmed using thin layer chromatography(TLC) and column chromatography, FT-IR, 1HNMR and 13CNMR spectral and were evaluatedforAnti-bacterial activity against Staphylococcus aureus, Pseudomonas aeruginosa, Escherichiacoli,Klebsiella pneumoniae and Bacillus subtilis and Anti-fungal activity against CandidaalbicansandAspergillus niger
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co-supervisor

EXTRACTION, CHARACTERIZATION OF UNRIPE BANANA STARCH COMPOSITE AND OKRA FIBRE REINFORCEMENT

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This study explores the extraction and characterization of starch composites derived from unripe banana (Musa spp.) reinforced with okra (Abelmoschus esculentus) fibre, with a focus on their structural, chemical, and mechanical properties. The starch was extracted from unripe bananas sourced from Evbuotubu, Benin City, while okra fibres were obtained from Oluku Market. Composite formulations were prepared by blending 10 g of banana starch with 3 g of okra fibre and plasticized using 5mL of glycerol. Fourier Transform Infrared Spectroscopy (FTIR) analysis confirmed enhanced hydrogen bonding interactions in the fibre-reinforced composite, evidenced by a stronger and slightly shifted O-H stretching peak (3300–3400 cm⁻¹) and the emergence of carboxyl (C=O) functionalities around 1700–1750 cm⁻¹. Elemental analysis revealed a decrease in carbon content from 70.02% (0G fibre) to 66.88% (3G fibre) and an increase in nitrogen from 23.40% to 29.56%, suggesting the introduction of nitrogen-rich organic components from okra fibre. The presence of calcium (0.48%) in the 3G fibre composite, absent in the 0G fibre sample, indicates mineral incorporation. Scanning Electron Microscopy (SEM) images showed a denser microstructure in the 0G fibre composite, whereas the 3G fibre composite exhibited a rougher and more porous texture, indicative of improved fibre-starch interfacial adhesion. Thermogravimetric Analysis (TGA) demonstrated enhanced thermal stability in the fibre-reinforced composite, with a higher degradation onset temperature and increased residual char content, confirming its resistance to thermal decomposition. X-ray Diffraction (XRD) patterns indicated a reduction in crystallinity upon fibre incorporation, as evidenced by broader and less intense diffraction peaks, suggesting a transition to a more amorphous structure. These findings demonstrate that okra fibre reinforcement significantly enhances the mechanical strength, thermal stability, and flexibility of starch composites, making them suitable for biodegradable applications in packaging and sustainable material development.
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co-supervisor

EVALUATION OF NUTRITIONAL VALUE OF GINGER (Zingiber officinale)

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The result for proximate analysis on Ginger( Zingiber officinale) showed carbohydrates 59.97± 0.41, crude fibre 3.65± 0.05, Ash 6.23 ± 0.10, Crude fat 8.66±0.35, protein 11.90 ±0.15 and moisture 9.47±0.09. From the results, ginger has high carbohydrate content and contain low value of moisture indicating a longer shelf life.The Phytochemical screening of ginger showed the presence of alkaloid, flavonoid, phenolics, terpenoids, saponin, glycoside,steroids and the absence of tannin, phlobotanin and anthraquinone. Antimicrobial, anti-oxidant, anti-inflammatory property can be attributed to the presence of the phytochemicals present.
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co-supervisor

POTASSIUM BROMATE LEVELS IN BREAD SOLD WITHIN BENIN CITY

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This study investigates the presence and concentration of potassium bromate in bread samples collected from various bakeries and retail outlets in Ovia North-East,Benin City,Edo State,using colorimetric detection and UV-Visible spectrophotometry.The qualitative analysis employed potassium iodide and hydrochloric acid to detect bromate presence through color changes ,while quantitative analysis utilized spectrophotometry to measure bromate levels accurately.The results revealed that potassium bromate concentrations ranged from (26.95 ± 17.33 µg/g) to (167.72 ±26.00 µg/g), with the highest levels found in Sample I (167.72 ± 26.00 µg/g) and Sample F (155.46 ± 25.96 µg/g), suggesting potential non-compliance with food safety regulations. Findings from this study provide valuable insights into the safety of locally available bread, highlight the need for stricter enforcement of food safety regulations, and raise consumer awareness about the dangers of potassium bromate, contributing to improved public health and regulatory oversight in the region
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co-supervisor

EVALUATION OF THE CHEMICAL COMPOSITION AND PHYTOCHEMICAL CONSTITUENTS OF TIGER NUT (Cyperus esculentus)

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This study evaluated the chemical composition and phytochemicals present in tiger nuts as a potential alternative to synthetic drugs with side effects. The result for proximate analysis of tiger nut (Cyperus esculentus) showed carbohydrate 50.89±0.25, crude fibre 7.50±0.29, crude protein 4.57±0.08, ash 3.00±0.29, crude fat 26.53±0.18 and moisture 7.50±0.29. From the result,
tiger nut contains high amount of carbohydrates and low moisture, indicating a good shelf life
Mineral analysis identified high levels of potassium (2565 mg/kg) and phosphorus (4914 mg/kg), along with significant amounts of magnesium (52 mg/kg) and iron (190 mg/kg). The phytochemical screening of tiger nut confirmed the presence of various bioactive compounds like glycosides, alkaloids, saponins, phenols, eugenols, terpenoids, and flavonoids, indicating
potential health benefits. The absence of tannins and steroids suggests minimal anti-nutritional factors. These findings provide valuable data on the nutritional and bioactive profile of tiger nuts, supporting their exploration as a natural source of health-promoting compounds.
Supervisor(s)
co-supervisor

SEED EXTRACT MEDIATED GREEN SYNTHESIS OF CALCIUM OXIDE NANOPARTICLES FROM SNAKE GOURD (Trichosanthes cucumerina) FOR PHYTOCHEMICAL SCREENING AND ANTIBACTERIAL INVESTIGATION

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In this research study, the preparation of Calcium oxide (CaO) nanoparticles (NPs) from Trichosanthes cucumerina seeds was reported to be synthesized by precipitation method using CaCl2 and NaOH as starting materials.The gradual change of the particles from pale yellow to a white precipitate indicated the formation of CaO nanoparticles The synthesized nanoparticle was subjected to characterization using Fourier Transform Infrared spectroscopy (FTIR), X-ray Diffraction (XRD) and Dynamic Light Scattering (DLS).The Phytochemical analysis of the CaO nanoparticles revealed that the aqueous extract was rich in phytochemicals as majority of the phytochemicals tested were positive which resulted in the rational support for the traditional use of T. cucumerina to cure wounds. T. cucumerina has antibacterial components that are effective against wound pathogens such as S. aureus, E. coli, B. cereus, K. pneumoniae, P. aeroginosa. The extracts displayed antibacterial activity against both gram (+) and gram (-) bacterial stain such as indicating the existence of a broad spectrum of antibacterial properties
Supervisor(s)
co-supervisor