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Thesis (M.S.)--University of Wisconsin--Madison, 1970. / eContent provider-neutral record in process. Description based on print version record. Includes bibliographical references.

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<p> Edible oils consist primarily of triacylglycerols (or TAGs), which are triesters of glycerol and fatty acids. Determination of the TAG compositions of edible oils is becoming more important, given the economic value of these oil products and the increasing incidence of adulterating high quality oils with poorer quality oils. In this study we report the development of an analytical protocol using positive ion infusion electrospray mass spectrometry (ESI/MS) in conjunction with tandem mass spectrometry which affords both identification and quantification of TAGs in edible oils samples.</p> <p> This thesis reports a simple, comprehensive and quantitative method for the analysis of TAGs in edible oils in which the optimized method involves the infusion of an oil sample in chloroform:methanol (1:1) solution (~10-15 μg/mL of oil) in the presence of 0.5 mM LiCl. A sequence of corrections were applied to the raw peak area data of the TAG molecular ions, [M+Li]+, to account for: (1) normalization of peak area data using three internal standards, (2) peak area contributions of M+2 isotopic peaks of TAGs with one more degree of unsaturation and (3) peak area contributions of LiCl adduct ions, [M+Li+LiCl]+, when applicable. The major correction involved multiplication to a given TAG peak area by the appropriate electrospray relative response factor (RRF) for that TAG. The RRFs for all TAGs containing between 48 and 63 carbons in their fatty acyl chains and between 0 and 9 degrees of unsaturation were extrapolated from experimentally determined response factors of a series of standards. The RRFs were found to decrease by 6.7% for each additional acyl chain carbon but increased by 18.6% for each double bond. Comparison of these calculated RRFs to reported RRFs for a series of TAG standards showed an excellent correlation (1.06% ± 10.20% RSD).</p> <p> The use of Li+ in TAG analysis followed from the reports by Hsu and Turk [93] and Han and Gross [18] which showed that Li+ afforded more intense MS, and particularly MS/MS, spectra than either H+ or Na+. The enhanced intensities in MS/MS spectra (determined using a triple quadrupole mass spectrometer) were critical for the identification of TAGs, including the identity of the fatty acyl group located at the sn-2 position. However, this method cannot distinguish unambiguously between isobaric TAGs. This methodology was applied to the profiling of a number of edible oils including canola, olive, sesame, grape seed, walnut and hemp seed oils. The major TAGS in these samples contained 52, 54 and 56 carbons with between 0 and 11 degrees on unsaturation in a given TAG. There were minor amounts of TAGs containing 50, 55 and 57 carbons.</p> <p> The ability of this method to determine quantitatively the number of degrees of unsaturation in an oil sample was tested by examining a series of partially hydrogenated canola oil samples kindly provided by Bunge Canada. Five oil samples derived from a single feedstock with differing numbers of degrees of unsaturation, measured as iodine values, were subjected to our analytical method. The measured iodine values were compared to iodine values calculated from the number of degrees of unsaturation obtained by our MS-based method. The slope of this correlation was 1.10 with an R^2 = 0.995. Overall, this method is much simpler and more accurate than the protocol described by Han and Gross [18]. This methodology will be applied as routine method for the analysis of TAGs in biological samples such as blood samples.</p> / Thesis / Master of Science (MSc)

It is estimated that over a third of the diet in the Western world is made up of oils and fats, of which a prominent percentage is in the form of emulsion food products, including milks, creams, yoghurts, margarines, salad dressings, desserts, soups and cheese. Current processing techniques involve the extraction and refining of edible oils using high temperatures and organic solvents, followed by re-encapsulation of the oil, for incorporation into the required emulsion products. The research presented in this PhD thesis was performed within the auspices of the UK Department of Environment, Food and Rural Affairs (DEFRA) funded, Sustainable Emulsion Ingredients through Bio-Innovation (SEIBI) project, which involved collaboration with researchers from the University of Nottingham together with a consortium of industrial partners. SEIBI was initiated to investigate a novel processing route for the production of food-grade rape and sunflowerseed oil emulsions from aqueously extracted oil-bodies. Being less energy and chemical intensive, the novel process offered potential reductions in both greenhouse gas emissions and wider environmental impacts when compared with conventional processing. Using Life Cycle Assessment (LCA) techniques, the environmental burdens of the aqueous oil-body extraction process were determined and compared with those of the existing technology route. To facilitate this, the research focussed on six key objectives, designed to both identify the environmental loads of the systems involved and scrutinise the impact of a number of methodological choices for LCA. These included choice of allocation method, normalisation, scaling issues distinct for novel processes and the extent to which the single-issue LCA variant, carbon footprinting could be used as an environmental indicator for the system. LCAs for four separate categories of product systems were developed encompassing seed oils, mayonnaises, aqueously extracted oil-body materials and mayonnaise-like oil-body emulsions. In addition to generating the environmental profiles required to fulfil the research objectives, the analysis of these models enabled the generation of original knowledge through the quantification of impacts for a range of processes that had either not previously been assessed or for which no published data could be found. The novel process was concluded as having clear potential for improved environmental performance over current technology even in its' pre-optimised, although the methodological choices examined were found to have profound effects on these and other results. Oil-body yield from seed was identified as key for optimisation to further maximise the environmental gains, with modest improvements, well within those theoretically possible being required for the novel process to better the environmental credentials of current technology in all key impact areas. The original outputs from this thesis will be of considerable use to developers involved in the continued advancement of the oil-body extraction technology, together with researchers within the edible oils and emulsions sector. In addition, the methodological outputs will help to inform LCA practitioners and developers in the continuing quest to understand the capabilities and limitations of this powerful analytical tool.

Alternative fuels are becoming important due to diminishing fossil fuel reserves and the environmental hazards associated with exhaust gases. Biodiesel is an attractive alternative fuel because it is environmentally friendly and can be synthesized from edible/non-edible oils. Though several methods are available for synthesis, transesterification is the preferred route for biodiesel synthesis. The current techniques for transesterification of the oils to biodiesel are based on acid/alkali catalysis. However, these methods do not work for oils with high free fatty acid content and also require an additional downstream step for separation of catalyst from the product. In this work, we investigate the synthesis of biodiesel by two techniques: in supercritical methanol and ethanol without any catalyst; in supercritical carbon dioxide using enzyme as catalyst. In the first technique, the transesterification of refined grade edible oil like sunflower oil, palm oil and groundnut oil, and crude non-edible oils like Pongamia pinnata and Jatropha curcas was investigated in supercritical methanol and ethanol without using any catalyst from 200 oC to 400 oC at 200 bar. The variables affecting the conversion during transesterification, such as molar ratio of alcohol to oil, temperature and time were investigated in supercritical methanol and ethanol. The conversion to biodiesel increased from 30-40% at a molar ratio of 10 to 80-85% at a molar ratio of 45 to 50. Very high conversions (96-97%) were obtained in supercritical methanol and ethanol within 30 minutes at 350 oC. The kinetics of the reaction was modeled, the rate coefficients and activation energies were determined. As an enzymatic transesterification in organic solvents is mass transfer limited, supercritical fluids are found to be a better alternative because of their gas like diffusivity. Among potentially interesting solvents for enzymatic synthesis, carbon dioxide is the most obvious choice in supercritical fluids, because it is non-toxic, nonflammable and easily available. Because the products and the enzyme do not dissolve in carbon dioxide at room conditions, separation can easily be achieved by reduction of pressure Thus, the enzymatic transesterification for production of biodiesel in supercritical fluids under mild conditions is of commercial interest. Therefore, biodiesel was synthesized using immobilized enzyme (Lipase, Novozym-435) in supercritical carbon dioxide. The effect of reaction variables like temperature, molar ratio, enzyme loading and kinetics of the reaction was investigated. The conversion to biodiesel was found to be lower in supercritical carbon dioxide than that in supercritical alcohol.

La presente investigación tuvo como objetivo general evaluar la calidad química de aceites de Sesamum indicum (ajonjolí) y Linum usitstissimum (linaza) que se expenden en dos Bioferias de los distritos de Miraflores y Barranco en Lima, Perú. Fue un estudio descriptivo de corte transversal. Se llevó a cabo en el laboratorio de bioquímica de alimentos de la Universidad Peruana de Ciencias Aplicadas (UPC), sede Villa en Chorrillos, y en el laboratorio Société Générale de Surveillance - SGS Perú, entre los meses de setiembre y octubre de 2018. Se realizaron distintas pruebas químicas a las muestras de aceite de ajonjolí y linaza: determinación de densidad, índice de acidez, acidez libre, índice de iodo e índice de peróxidos; a estas se le sumaron la evaluación de las condiciones de almacenamiento, del etiquetado y del registro sanitario. De acuerdo con los resultados obtenidos podemos indicar que en términos generales los aceites de linaza y ajonjolí de las marcas analizadas que se expenden en las Bioferias de Miraflores y Barranco se encontraban fuera de los rangos establecidos en por lo menos un indicador químico, tomando como parámetro de contrastación la Norma CODEX (STAN 210-1999) para aceites comestibles. / The general objective of this research was to evaluate the chemical quality of Sesamum indicum (sesame) and Linum usitatissimum (flax) seed oils sold in two Biofairs of the districts of Miraflores and Barranco in Lima, Peru. This was a descriptive, cross-cutting study. Analyses were made in the laboratory of food biochemistry of Universidad Peruana de Ciencias Aplicadas (UPC), campus of Villa in Chorrillos, and in the laboratory of Société Générale de Surveillance - SGS Peru, in the months of September and October 2018. Different chemical tests were performed to the sesame and flax seed oils to measure: density, acidity, free fatty acid, iodine and peroxide values. Additionally, storage conditions, labeling and sanitation registration were also evaluated. According to the results obtained, we can state that in general terms flax and sesame seed oils of the analyzed trademarks sold in the Biofairs of Miraflores and Barranco were out of the ranges established in at least one chemical indicator, taking CODEX standard for edible oils (STAN 210-1999) as the reference standard. / Tesis

Este trabalho teve como objetivo a síntese e caracterização de sílicas mesoporosas suportadas com níquel para atuarem como catalisadores na hidrogenação de óleos vegetais. Foram escolhidas as sílicas mesoporosas ordenadas do tipo SBA-15 e FDU-1, sintetizadas a partir de TEOS como fonte de sílica e copolímeros triblocos como agentes direcionadores de estrutura em meio HCl. O Ni(NO3)2.6H2O foi utilizado como fonte de metal, cuja solução aquosa com a concentração de níquel desejada foi adicionada à sílica antes da remoção do molde polimérico, originando os precursores dos catalisadores. Após a impregnação, as amostras foram submetidas à calcinação sob atmosfera de ar, gerando o precursor na forma de óxido que ao ser tratado com H2 é reduzido Nio , forma ativa do catalisador. As técnicas de termogravimetria, termogravimetria derivada, difração de raios X a alto e baixo ângulo, isotermas de adsorção de nitrogênio e absorção atômica foram empregadas para a caracterização destes materiais. A TG/DTG foi utilizada para a simulação das melhores condições de calcinação/redução. As amostras foram calcinadas em um forno tubular com controlador de temperatura. Os ensaios de DRX confirmaram a fase NiO após calcinação e a fase Nio na redução, por termogravimetria. A difração por raios X, confirmou a presença da fase Ni . Os resultados dos ensaios de difração de raios X a baixo ângulo indicaram que com teores de Ni de até 10%, não há modificação na estrutura dos materiais SBA-15 e FDU-1. As isotermas de adsorção de nitrogênio são do tipo IV, características de materiais mesoporosos. Os teores de níquel foram medidos por absorção atômica. Os valores de áreas superficiais dos materiais com 10% de Ni foram superiores a 300 m2 /g, sugerindo que tais materiais são promissores para prosseguir com os estudos e efetivamente testá-los como catalisadores na hidrogenação de óleos vegetais / This work aimed at the synthesis and characterization of mesoporous silica supported with nickel to act as catalysts in the hydrogenation of vegetable oils. The SBA-15 and FDU-1 were chosen as mesoporous ordered silica types, synthesized from TEOS as a source of silica and tribloco copolymers as molded agents of the structure in the midst HCl. The Ni(NO3)2.6H2O was used as a source of metal, whose aqueous solution with the desired concentration of nickel has been added to the silica before the removal of mold polymer, forming the catalytic precursors. After impregnation, the samples were subjected to calcination under air atmosphere, creating the precursor in the oxided form which being treated with H2 is reduced to Nio , active form of the catalyst. The TG techniques, thermogravimetric derived, X-ray diffraction at high and low angles, nitrogen adsorption isotherms, and atomic absorption spectrometry were used to characterize these materials. The TG / DTG were used for the simulation of best calcination / reduction conditions. The samples were calcined in a tubular oven with temperature controller. The DRX tests confirmed the NiO phase after calcination and Nio phase in the reduction by TG. The SAXS results indicated that Ni levels up to 10% do not change the material structures such as SBA-15 and FDU-1. The nitrogen adsorption isotherms are the IV type, characteristics of mesoporous materials . The nickel levels were measured by atomic absorption spectrometry. Surface area values for materials with Ni10% were greater than 300 m2 / g, suggesting that such materials are promising to proceed with the studies and test them effectively as catalysts in the hydrogenation of vegetable oils

Orientador: Antonio Jose de Almeida Meirelles / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-12T23:48:24Z (GMT). No. of bitstreams: 1 Cren_ErikaCristina_D.pdf: 3396631 bytes, checksum: 2aba05c13e0a564804083d131df53687 (MD5) Previous issue date: 2009 / Resumo: Alguns óleos vegetais são sensíveis às condições drásticas do processo de refino, físico ou químico, podendo assim apresentar problemas quando submetidos a estes processos, tais como perda de substâncias desejáveis, como os compostos nutracêuticos, escurecimento do óleo, além de perdas elevadas de óleo neutro. Desta forma a busca de alternativas no processamento de óleos vegetais se torna relevante. O processo de extração líquido-líquido vem sendo estudado como alternativa para a desacidificação destes óleos vegetais, pois utiliza condições brandas de processo. No entanto, esta técnica apresenta a desvantagem de demandar grandes volumes de solvente para a extração, havendo a necessidade de recuperação do solvente usado para sua futura reutilização. As resinas de troca iônica vêm sendo utilizadas em muitos segmentos da indústria de alimentos, para separação e purificação de ácidos orgânicos. Assim, resinas de troca iônica e de adsorção podem ser empregadas como complemento da extração líquido-líquido, em particular na remoção de ácidos graxos da corrente de extrato e na recuperação do solvente para sua reutilização posterior. Contudo, identifica-se também um potencial uso da resina de troca iônica na desacidificação direta de óleos vegetais brutos, sugerindo assim uma nova alternativa à desacidificação de óleos vegetais sensíveis às condições dos refinos tradicionais, uma vez que este processo também opera em condições brandas como a extração líquido-líquido, porém não necessita de grandes volumes de solvente para a desacidificação. Além disso, esta nova alternativa de refino permite que parte do solvente utilizado na extração de óleo da semente, polpa ou farelo, possa ser utilizada como solvente do processo de troca iônica, podendo ser misturado a outros solventes ou até mesmo substituído por outros na extração de óleo, uma vez que estudos vêm sendo feitos para substituir o hexano da extração devido à sua periculosidade. Este novo processo ainda visa reciclar todo o solvente utilizado para posterior reutilização no processo de refino. A nova alternativa também pode gerar eliminação de algumas etapas do processo tradicional de refino de óleos, uma vez que na proposta o hexano da extração pode ser parcialmente utilizado na troca iônica e eliminado completamente do óleo neutro em apenas uma coluna de destilação que pode operar a até 140o C, condição branda para alguns óleos nos quais se quer preservar características nutracêuticas. Sendo assim, este trabalho teve por objetivo estudar sistemas modelo que simulassem a corrente de extrato da extração líquido-líquido (etanol + acido oléico) e sistemas modelo que simulassem uma corrente de saída da extração de óleos vegetais (solventes butanol e/ou hexano + ácido oléico e solventes butanol e/ou hexano + ácido oléico + óleo vegetal), quanto à capacidade da resina de troca iônica remover a acidez livre daquelas correntes. Desta forma, os comportamentos destes sistemas em resina de troca iônica foram investigados. Foram realizados estudos de equilíbrio, cinética e em coluna (sistema contínuo), com respectivas modelagens a fim de obter parâmetros que descrevessem o comportamento de troca iônica para os sistemas propostos. Bons resultados foram obtidos, demonstrando o potencial para uso da resina para os fins propostos. Por fim, uma nova alternativa de processamento de óleos pode ser formulada empregando-se resinas de troca iônica / Abstract: Some edible oils are sensitive to the drastic conditions of the caustic and physical refining, some difficulties arise when such processes were used, like losses of neutral oil and nutraceutical substances. In this way, the investigation of new alternatives of processing edible oils is relevant. The liquid-liquid process has been investigated as alternative for the deacidification of such oils, because it uses mild conditions of processing. But this process has the disadvantage of demanding large amounts of solvent for the extraction, so that the solvent needs to be recovered for posterior utilization. Ion exchange resins have been used in many areas, for purification and separation of organics acids. In this way, it could be used as a complement of the liquid-liquid extraction, for removing fatty acids from the extract stream and recovering the solvent for posterior use. A potential use of ion exchange resins to directly deacidify crude oil was also identified, so a new alternative to the deacidification of edible oils that are sensitive to the drastic conditions of traditional refining was proposed. This new alternative of refining can use the solvent (hexane) employed in the extraction of the oil as solvent of the ion exchange process. This solvent could be mixed with other solvents or substituted by other less dangerous. In this new process a further objective is the recovery of all solvent used for posterior reutilization. This new process could eliminate some steps of the traditional refining, once that the hexane could be used partially on the ion exchange process and eliminate from the refined oil in only one stage, in mild conditions that preserve the nutraceutics characteristics of some oils. In this way, this work has as objectives the investigation of the deacidification by ion exchange resins of systems that simulate the extract of liquid-liquid extraction (ethanol + oleic acid) and systems that simulate the outlet stream of oil extraction from the seeds (solvent butanol or/and hexane + oleic acid and solvent butanol or/and hexane + oleic acid + rice oil). So the behavior of these systems in ion exchange resins was investigated. Experimental studies of equilibrium, kinetics and breakthrough were conducted and an appropriate modeling of the experimental results was also performed. The objective was to determine the parameters that describe the process of ion exchange for investigating the viability of using ion exchange resins in new processes of refining. Good results were obtained, indicating the possibility of using ion exchange resins for removing fatty acids from organic solutions / Doutorado / Doutor em Engenharia de Alimentos