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Item PHYTOCHEMICAL AND PHARMACOLOGICAL EXAMINATION OF ENTANDROPHRAGMA ANGOLENSE AND CRYPTOLEPIS SANGUINOLENTA(1994-03) KOLAWOLE, A. J.Dried, pulverized stem bark and the root bark of Entandrophragma anqolense were separately extracted with methanol. The crude methanolic extract of the stem and root bark of E. anqolense were subjected to column fractionation and purification. This exercise afforded the Isolation of methyl angolensate, 2.26% yield from the stem bark and 0.27% yield from the root bark. The effect of the crude methanolic stem bark extract was investigated on indomethacin-induced gastric ulcer in rats. Its effect was dose-dependent, doses ranging from 0.4 to 1.6 gkg-1 body weight (BW) produced significant effect (P < 0.05). At the highest dose used (1.6gkg-1 BW), complete inhibition of ulceration occurred. Toxicity study showed that the extract was not toxic when doses ranging from 20-200gkg-1 BW was administered to experimental rats. It was established that methyl angolensate is the major anti- ulcer principle present in the methanolic extract of the stem bark of E. angolensate. Methyl angolensate produced a dose-related inhibition of gastric ulceration induced by indomethacin, 40mgkg BW being more effective than 40mgkg-1 BW of propanolol. 80mgkg-1 BW of methyl angolensate completely inhibited gastric ulceration. Methyl angolensate also significantly reduced gastric acid secretion induced by histamine and carbachol (1.0mgkg-1 BW). Thus we confirmed that methyl angolensate produces its anti-ulcer activity through inhibition of gastric acid secretion. The roots of Cryptolepis sanquinolenta were extracted with methanol. Column fractionation of the methanolic extract afforded the Isolation of a new benzocarboline alkaloid labelled (CS-1) melting point 272-274°C. Spectroscopic analysis of CS-1 including the infra-red (IR), 13 ultra-violet (UV), mass spectrum (MS), proton and C-nuclear magnetic spectroscopy were reported. This new alkaloid exhibited anti-microbial activity on five pathogenic organisms. The in-vivo anti-malarial study of the aqueous extract of the roots of sanguinolenta was done on Plasmodium yoeli nigeriensis in mice. Anti-malarial activity of the extract was determined by examining the blood schizontocidal action in established infection using chloroquine as Standard drug for comparison. The extract showed a dose-dependent effect against the malarial parasite.Item DESULPHURIZATION OF NIGERIAN LAFIA COAL FOR METALLURGICAL COKE PREPARATION(1988-01) ADERONPE, W. I. A.The Government-owned integrated iron and steel plant under construction in Ajaokuta has been designed to operate through the blast-furnace process. The blast-furnace requires metallurgical coal. It therefore became necessary and relevant to the national economy to scientifically work on Nigerian coals with a view to using same as metallurgical coal. Lafia coal is the only Nigerian coal that produces coke lump after dry distillation (carbonization). The property of coke- ability therefore attracted attention towards Lafia coal. The main interest was to so prepare the coal that as much as possible of it will be usable for metallurgical coke preparation for use in Ajaokuta blast-furnace. Lafia coal was subjected to chemical characterization and petrological studies. It became clear that it was high in ash and sulphur. Silicates, pyrites and carbonates of various elements constituted the inorganic mineral inclusions. Analytical data gave the sulphur varieties in Lafia coal to be organic (0.1 - 0.7%), pyritic (1.4 - 4.4%) and sulphate (0.01 - 0.07%). Pyritic sulphur which predominates in Lafia coal can be removed by physical means. Chemical desulphurization which is reducto-oxidative type of chemical reaction impares coal cokeability. A plunge was thus made for physical desulphurization techniques to bring down the total sulphur in Lafia coal to the level that will make it acceptable as a metallurgical coal with regards to its sulphur content. Trace elements in Nigerian coal ash determined using the Atomic Absorption Spectrophotometer (AAS) and confirmed with the Inductively Coupled Plasma Emission Spectrophotometer (ICPES) showed that the relative abundance of the elements in the coals depended on the biogeo-chemistry of the area of the deposit as follows: Lafia coal; F>Zn>Mn»V Cr>Ni>Cu>B>Pb>Ca>Be>Mo>Cd>Hg Enugu coal; B>Mn>V F>Cr>Zn>Cu>Pb Ni>Co>Be>Mo>Hg Okaba coal; Mn»B»V>Cr>Cu>Pb>F=Ni>Zn Co>Be>Mo>Hg Trace element content of coal was considered in connection with the impact of coal utilization on the environment. From the study it was concluded that either the wet concentrating table or the froth flotation method could be used to substantially desulphurize Lafia coal to meet the requirement of metallurgical coal.Item DEVELOPMENT OF RESIN-BOUND REAGENTS FOR ANALYSIS OF CARBOXYLIC ACIDS AND AMINES(1993-12) ADEWUYI, G. O.Resin-bound-reagents made up of ionically-bound 2- naphthalene-methanol and covalently bound and sodium-benzoxazole- 2-sulfonate have been synthesized and utilized as analytical reagents for the pre-chromatographic derivatization of fatty acids (i.e. acetic, lauric, capric, hexanoic, octanoic, nonanoic, palmitic, docosanoic linoleic), 1° and 2° aliphatic amines and amino acids respectively. The reagents have been designed to contain fluorescent moieties attached to the anionic and cationic resin backbones through sulfonated ester linkages. These moieties imparted UV and FL detector properties to the final derivatives. The derivatization reactions were performed before the thin- layer Chromatographie separations. Standards we,-e prepared and were used in monitoring the extent of reactions on the resin support. The derivatives were chromatographed and fluorescent spots were observed under UV light. These solid phase derivatizations have led to preliminary investigation of these two functionalities before embarking on instrumentation analysis such as high performance liquid chromatography with UV or fluorescence detection and HPLC-MS Identification.Item METAL(II) TETRAFLUOROBORATE COMPLEXES OF SOME DICARBOXYLIC ACID HYDRAZIDES(1990) ADENIYI, A. A.Eighty-eight divalent metal complexes derived from dihydrazides of oxalic, malonic, succinic, adipic, phthalic and terephthalic acids, with manganese( 11), cobalt(ll), nickel(ll), copper(IJ), zinc(ll), cadmium(ll), mercury(ll) and magnesium tetrafluoroborates have been prepared. The effect of 1:1 and 1:2 metal to ligand reactant ratios have been examined. The complexes have been characterized on the basis of their analytical data, magnetic susceptibility, electronic and IR spectral studies as well as conductance measurements. Reactions involving 1:1 and 1:2 metal to ligand ratios gave complexes with different metal to ligand stoichiometry in most cases. It is evident, from the analytical data, that complexes precipitated out mostly with 1:2 and 1:3 metal to ligand stoichiometry. However, complexes of oxalic dihydrazide with Cu (II) and Hg (II), succinic dihydrazide with Co (II), Ni(ll), Zn(ll) and Mg prepared using a 1:1 molar reactant ratio contained one and a half moles of ligands. Similarly, complexes of Mn(ll), Ni(ll) and Hg(ll) prepared using a 1:2 molar ratio of metal salt to adipic dihydrazide contained one and a half moles of adipic dihydrazide. Nevertheless, reactions involving 1:1 and 1:2 molar reactant ratios gave the same set of compounds in phthalic dihydrazide with Co(ll), Ni(ll) and Zn(ll) tetrafluoroborates respectively. Likewise the complexes of adipic and malonic dihydrazides with Zn(BF4)2 .6H2O4 and Cd(BF4)2 .7H2O respectively. The complexes have poor solubilities in methanol, ethanol, acetone, nitrobenzene, nitromethane, benzene, hexane, aceto- nitrile, dimethylformamide, dimethylsulfoxide and water. But the complexes of inanganese( 11), cobalt(ll), zinc(ll) and cadmium(II) with oxalic, malonic, succinic and adipic dihydrazides were found to be soluble in water. Similarly, nickel(11), CO ppe-f (11) and magnesium complexes of malonic and succinic dihydrazides were soluble in water, so also is the complex of mercury(ll) with adipic dihydrazide. In addition, the complexes of succinic dihydrazide, with manganesef11) and cadmium(ll) tetrafluoroborates were soluble in dimethylsulfoxide. The infrared spectra indicate that the bonding sites in these compounds are the carbonyl oxygen and the amino or amide nitrogens. The electronic and magnetic data of the complexes of manganese( 11), cobalt(ll), nickel(ll) and copper(ll) at room temperature suggested that they assume octahedral geometry. Generally, for a given ligand, the 1:2 complex has a lower magnetic moment than the 1:3 complex. The Variation of the moments with chain length does not appear to be systematic at room temperature. However, the magnetic moments for the Zn (11), Cd(II), Hg(ll) and Mg indicates that they are diamagnetic with some evidence of polarization paramagnetism. The conductance data of the complexes that were soluble in water and dimethylsulfoxide revealed 1:2 type electrolytes.