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Biocatalytic Production, Preparation and Characterization of Large-ring CyclodextrinsMokhtar, Mohd Noriznan 26 January 2009 (has links)
Cyclodextrins (CD) are cyclic oligosaccharides composed of six to more than sixty
glucose units. Large-ring cyclodextrins (LR-CD) are novel CD comprised of more than eight
glucose units with cavity structures and sizes different from that of commercially available
CD<sub>6</sub> – CD<sub>8</sub>. LR-CD may offer unique molecular recognition properties and can be produced
biocatalytically from starch using cyclodextrin glucanotransferase (CGTase, E.C. 2.4.1.19) in
a short reaction time. LR-CD were isolated from glucose, CD<sub>6</sub> – CD<sub>8</sub> and other compounds by
complexation of CD<sub>6</sub> – CD<sub>8</sub> as well as precipitation techniques. The yield of LR-CD (degree
of polymerization from 9 to 21) was optimized using central composite design. Addition of
polar organic solvents to the synthesis resulted in higher yields of LR-CD. LR-CD composed
of 9 to 21 glucose units were successfully separated using reversed-phase of ODS-AQ
chromatography and normal-phase of polyamine II chromatography. Maintaining optimized
reaction conditions aided in a high yield of CD<sub>9</sub>; it could be separated with reasonable yield
using a single step of polyamine II chromatography. A co-grinding method helped to obtain
higher solubilization levels of glibenclamide, vitamin A acetate and vitamin D<sub>3</sub> in CD<sub>13</sub>, CD<sub>10</sub>
and CD<sub>11</sub>, respectively when compared to other CD. Vitamin K<sub>1</sub> was solubilized in distilled
water with CD<sub>6</sub> – CD<sub>13</sub> using a co-precipitation method. When compared with other CD, CD<sub>9</sub>
was seen to be the best solubilizer. The analysis of complexes using ESI MS showed
spironolactone and glibenclamide complexed with CD<sub>9</sub> and CD<sub>13</sub>, respectively.
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[en] PRODUCTION AND CHARACTERIZATION OF MAGNETITE STRUCTURES: NANOPARTICLES, THIN FILMS AND LITHOGRAPHED ARRAYS / [pt] PRODUÇÃO E CARACTERIZAÇÃO DE ESTRUTURAS DE MAGNETITA: NANOPARTÍCULAS, FILMES FINOS E PADRÕES LITOGRAFADOSGERONIMO PEREZ 29 October 2021 (has links)
[pt] Este trabalho pode ser dividido em três etapas principais: síntese das nanopartículas, deposição de filmes finos e litografia por feixe de elétrons. As nanopartículas magnéticas foram sintetizadas pelo método de co-precipitação a partir de sulfato de ferro II (FeSO4), cloreto férrico (FeCl3) e hidróxido de amônia (NH4OH) à temperatura ambiente. Para prevenir a formação de agregados, foi adicionado nitrato de sódio (NaNO3) em pequenas quantidades, que se mostrou bastante eficiente. Em seguida foram produzidos filmes de magnetita utilizando o sistema de pulverização catódica usando fonte de radiofrequência (sputtering RF). Os alvos foram produzidos por compactação das nanopartículas de magnetita produzidas anteriormente. Os filmes finos foram depositados em substrato de silício. A formação de magnetita durante a deposição foi confirmada por difração de raios-x e magnetômetro de amostra vibrante. Uma vez controlados os parâmetros de deposição, foram produzidos arranjos de magnetita. A litografia por feixe de elétrons foi produzida em substrato de silício recoberto com máscara de PMMA (polimetilmetacrilato) de 250 nm de espessura. Foram produzidos arranjos periódicos de formas básicas a modo de testar a técnica de litografia: quadrados de 1 μm e círculos de 1 μm, 500 nm e 250 nm de diâmetro formados de um filme de magnetita de 80 nm de espessura. A espessura do filme, forma, tamanho e separação das figuras que compõem os padrões litografados influenciam na facilidade com que será retirada a mascara de PMMA. / [en] This work can be divided into three main steps: synthesis of nanoparticles, thin film deposition and electron beam lithography. The magnetic nanoparticles were synthesized by co-precipitation method from iron II sulfate (FeSO4), ferric chloride (FeCl3) and ammonium hydroxide (NH4OH) at room temperature. A small amount of sodium nitrate (NaNO3) was added to avoid the cluster formation, which was very efficient. Then the magnetite thin films were produced using the sputtering RF (radio frequency source) system. The targets were produced by compression of magnetite nanoparticles previously produced in the first step. The thin films were deposited on a silicon substrate. The formation of the magnetite after the deposition was confirmed by x-ray diffraction and vibrating sample magnetometer. The arrays of magnetite were made once the deposition parameters were controlled. The electron beam lithography has been produced on silicon substrate covered of PMMA (polymethylmethacrylate) resist 250 nm thick. Were produced periodic arrays of basic forms a way to test the technique of lithography, a square micron circles 1 μm, 500 nm and 250 nm in diameter formed of a magnetite film 80 nm thick. The film thickness, shape, size and separation of the figures which comprise standards lithographed can influence the ease with which the mask is withdrawn from PMMA.
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