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(1 - 6 of 6)
- Title
- ATTEMPTS TO SYNTHESIZE A PORPHYRIN CONTAINING A FUSED CYCLOALKANO RING SYSTEM.
- Creator
- GUTIERREZ HERNANDEZ, GUSTAVO A., Florida Atlantic University
- Abstract/Description
-
The ensuing treatise details the routes investigated in the attempt to synthesize a novel porphyrin related to deoxophylloerythroetioporphyrin (DPEP), containing a fused six-membered cycloalkano ring system and a carboxylic acid chain in its structure. Mesorhodin methyl ester, the intermediate used throughout this study was obtained from mesoporphyrin dimethyl ester which in turn, was prepared from hemin. Attempts to reduce the keto-function in mesorhodin methyl ester to the corresponding...
Show moreThe ensuing treatise details the routes investigated in the attempt to synthesize a novel porphyrin related to deoxophylloerythroetioporphyrin (DPEP), containing a fused six-membered cycloalkano ring system and a carboxylic acid chain in its structure. Mesorhodin methyl ester, the intermediate used throughout this study was obtained from mesoporphyrin dimethyl ester which in turn, was prepared from hemin. Attempts to reduce the keto-function in mesorhodin methyl ester to the corresponding methylene group in our target coumpound were based on two methods. The first approach was application of the Huang-Minlon modification of the Wolff-Kischner reaction. The second procedure considered chemical and catalytic hydrogenations as well as dehydration reactions. Although our proposed pathways were found to be unsatisfactory, the latter methodology did lead to unreported intermediates and a new porphyrin with a fused benzene ring. Their syntheses and spectral properties are discussed.
Show less - Date Issued
- 1986
- PURL
- http://purl.flvc.org/fcla/dt/14339
- Subject Headings
- Porphyrins
- Format
- Document (PDF)
- Title
- Vanadyl and nickel geoporphyrin biodegradation study in high sulfur Monterey crude oils and Canadian tar sands.
- Creator
- Magnier, Clotilde Caroline, Florida Atlantic University, Baker, Earl W.
- Abstract/Description
-
Oil samples from the Monterey formation (California) and McMurray (Canada) formations have been analysed in order to relate bacterial biodegradation and metallo-porphyrins found in crude oils. The choice of samples was made according to biodegradation levels, in order to relate these processes with pigment degradation. Vanadyl and nickel petro-porphyrins were isolated by column chromatography, analyzed by Mass Spectrometry, and were correlated to maturity with DPEP to ETIO ratios and plots of...
Show moreOil samples from the Monterey formation (California) and McMurray (Canada) formations have been analysed in order to relate bacterial biodegradation and metallo-porphyrins found in crude oils. The choice of samples was made according to biodegradation levels, in order to relate these processes with pigment degradation. Vanadyl and nickel petro-porphyrins were isolated by column chromatography, analyzed by Mass Spectrometry, and were correlated to maturity with DPEP to ETIO ratios and plots of %DPEP vs. alkylation indices. Experimental data indicates that (1) biodegradation and maturity are two independent chemical processes, and (2) that biodegradation does not affect the vanadyl porphyrin profile, thus making them excellent indicators of pre-biodegradation thermal histories for the source bitumen.
Show less - Date Issued
- 1991
- PURL
- http://purl.flvc.org/fcla/dt/14722
- Subject Headings
- Porphyrins--Biodegradation
- Format
- Document (PDF)
- Title
- Oxygen Exchange Studies and Resolution Attempts With Vanadyl Etioporphyrin I.
- Creator
- Pettersson, Berno I., Bieber, Theodore I., Florida Atlantic University
- Abstract/Description
-
Vanadyl etioporphyrin I has C4 symmetry and is chiral. Hence, it should be resolvable. Attempts were made to resolve it into its enantiomers by chromatography using optically active ads or bents since it has no functional groups which can be used to form isolable diastereomers. Numerous optically active ads or bents were tried in the pure state and adsorbed on silica gel. In most cases the Rf values were either close to zero or close to one, making resolution impossible. Only in the case of...
Show moreVanadyl etioporphyrin I has C4 symmetry and is chiral. Hence, it should be resolvable. Attempts were made to resolve it into its enantiomers by chromatography using optically active ads or bents since it has no functional groups which can be used to form isolable diastereomers. Numerous optically active ads or bents were tried in the pure state and adsorbed on silica gel. In most cases the Rf values were either close to zero or close to one, making resolution impossible. Only in the case of lactose on silica gel and using benzene as the solvent was the Rf value such (approx. 0. 52) that resolution seemed, at least, possible. However, no optically active fraction could be obtained on column chromatography. Since oxygen exchange between the vanadyl group of vanadyl etioporphyrin I and water might occur and cause rapid interconversion of the enantiomers (hence racemization), thereby vitiating resolution attempts, the possibility of such oxygen exchange was investigated under a variety of conditions by means of H2 O^18 . The I. R. method was used to detect any such exchange (VO^18 vs. VO^16). It was found that vanadyl etioporphyrin I fails to undergo any measurable exchange under all the conditions tried, although the vanadyl ion of vanadyl sulfate does undergo exchange.
Show less - Date Issued
- 1969
- PURL
- http://purl.flvc.org/fau/fd/FA00000808
- Subject Headings
- Porphyrins, Vanadium, Ferrocene, Chromatographic analysis
- Format
- Document (PDF)
- Title
- High performance liquid chromatographic separation of sedimentary vanadyl porphyrins.
- Creator
- Huang, Xiaoxue, Florida Atlantic University, Baker, Earl W., Charles E. Schmidt College of Science, Department of Chemistry and Biochemistry
- Abstract/Description
-
A method of reversed phase HPLC gradient elution was developed and evaluated for the separation of vanadyl porphyrins. Separation was compared with the result of isocratic elution. It shows that gradient elution method is suitable for vanadyl porphyrin separation and better separation result can be obtained by gradient elution. Gradient elution improves the separation by changing the retention time of different components in the sample mixture and increases the difference of k' (capacity...
Show moreA method of reversed phase HPLC gradient elution was developed and evaluated for the separation of vanadyl porphyrins. Separation was compared with the result of isocratic elution. It shows that gradient elution method is suitable for vanadyl porphyrin separation and better separation result can be obtained by gradient elution. Gradient elution improves the separation by changing the retention time of different components in the sample mixture and increases the difference of k' (capacity factor). Vanadyl porphyrin samples Bakken 6362', Treibs #1 and Treibs #3 were analyzed by this method. Results correlate very well with the results of mass spectrometry analysis of these samples which have been done by some other workers.
Show less - Date Issued
- 1994
- PURL
- http://purl.flvc.org/fcla/dt/15094
- Subject Headings
- Porphyrins, High performance liquid chromatography
- Format
- Document (PDF)
- Title
- HPLC separation and characterization of nickle geoporphyrins.
- Creator
- Zeng, Shaochuan, Florida Atlantic University, Baker, Earl W.
- Abstract/Description
-
HPLC separation of nickel geoporphyrin homologues and isomers has been markedly enhanced by a number of modifications of previously disclosed methods. A general, more efficient and reproducible method has been developed. A C18 3-micron reverse phase column with a programmed gradient binary mobile phase composed of solvent A which is methanol, water and solvent B which consists of methanol modified by the addition of powerful ligand; a consistent ratio of organic salt is added into this...
Show moreHPLC separation of nickel geoporphyrin homologues and isomers has been markedly enhanced by a number of modifications of previously disclosed methods. A general, more efficient and reproducible method has been developed. A C18 3-micron reverse phase column with a programmed gradient binary mobile phase composed of solvent A which is methanol, water and solvent B which consists of methanol modified by the addition of powerful ligand; a consistent ratio of organic salt is added into this solvent system to increase ionic strength of mobile phase. Straightforward HPLC separations of some marine sediment and oil shale extracts (nickel porphyrins) without demetallation have been successfully achieved. Most attention has been focused on Cowboy Gilsonite and Bakken oil-shale. Individual fractions have been collected and analyzed by UV-VIS, NMR, Mass spectrometry. Known compounds were used for co-chromatographic and spectroscopic reference.
Show less - Date Issued
- 1992
- PURL
- http://purl.flvc.org/fcla/dt/14880
- Subject Headings
- High performance liquid chromatography, Porphyrins
- Format
- Document (PDF)
- Title
- Synthesis and characterization of group IVB metallocene materials derived from hematoporphyrin IX.
- Creator
- Rivalta, Alberto Enrico., Florida Atlantic University, Carraher, Charles E., Haky, Jerome E.
- Abstract/Description
-
New organometallic containing materials were synthesized by the reaction of Group IVB metallocene dichlorides of the form Cp2MCl2 where M = Ti, Ar, and Hf with Hematoporphyrin IX using the interfacial condensation polymerization technique. The structural characterization was accomplished using infrared and mass spectroscopy and elemental analysis. The results obtained from these techniques showed the presence of the metal ester and ether bonding as evidence that the reaction occurred. The...
Show moreNew organometallic containing materials were synthesized by the reaction of Group IVB metallocene dichlorides of the form Cp2MCl2 where M = Ti, Ar, and Hf with Hematoporphyrin IX using the interfacial condensation polymerization technique. The structural characterization was accomplished using infrared and mass spectroscopy and elemental analysis. The results obtained from these techniques showed the presence of the metal ester and ether bonding as evidence that the reaction occurred. The product derived from titanocene dichloride, 12-A, exhibited growth inhibition characteristics towards the Candid albicans and Staphylococcus aureus microorganisms. From the preliminary metal adsorption studies it was shown that this product also bound nickel ions.
Show less - Date Issued
- 1993
- PURL
- http://purl.flvc.org/fcla/dt/14940
- Subject Headings
- Organometallic chemistry, Porphyrins, Hematoporphyrin, Metallocenes
- Format
- Document (PDF)
