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Development of microplasmas and analysis of complex biomolecules using plasma and synchrotron radiationSymonds, Joshua M. 27 August 2014 (has links)
In this work, a microplasma-based ionization source for ambient mass spectrometry (AMS) has been developed. Optical emission spectroscopy, optical microscopy, and electrical measurements have been used to characterize the discharge. The discharge was used in a direct exposure mode in AMS experiments, and was found to behave as a small Penning ionization source capable of ionizing a range of biomolecules via proton transfer. In order to broaden the effectiveness of the microplasma ionization source, admixtures of hydrogen in neon gas were used to produce vacuum ultraviolet (VUV) light. The 121.6 nm Lyman-? (10.23 eV) photons produced are effective soft (non-destructive), single-photon ionization sources. Since this photon energy exceeds the ionization potential of many biomolecules, this source is useful for analysis of a wide range of organic samples.
The microplasma source, in both VUV-generating and direct-exposure modes, is proposed as a method by which to study the damage effects on biomolecules, and preliminary results are presented.
Finally, a collaborative work investigating the role of ionizing radiation in the DNA damage process is presented. Using a synchrotron radiation source, the photolysis of DNA monolayers on gold substrates in a vacuum environment were studied by X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS) experiments.
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Development of Liquid Sample Holding Devices for Ambient Mass SpectrometryWu, Su-yuu 19 July 2010 (has links)
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Development of Ambient Mass Spectrometry for the Detection of Volatile Components from Liquid or Solid SamplesChen, Liang-Tsuen 15 July 2007 (has links)
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Monitoring of biodiesel oxidative degradation by traditional analytical methods and mass spectrometry : Monitoramento da degradação oxidativa do biodiesel por métodos analíticos tradicionais e espectrometria de massas / Monitoramento da degradação oxidativa do biodiesel por métodos analíticos tradicionais e espectrometria de massasPereira, Gustavo das Graças, 1983- 11 September 2018 (has links)
Orientador: Daniel Barrera Arellano / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-09-11T21:24:35Z (GMT). No. of bitstreams: 1
Pereira_GustavodasGracas_D.pdf: 2179143 bytes, checksum: 1e7fcb8f754269f187b842007445023a (MD5)
Previous issue date: 2015 / Resumo: A utilização do biodiesel na matriz energética brasileira apresenta diversas vantagens tecnológicas, ambientais e sociais. Entretanto, é importante salientar que esse biocombustível é menos estável ao armazenamento quando comparado ao diesel. Nesse contexto, o objetivo desse trabalho consistiu em estudar o comportamento de oxidação do biodiesel utilizando métodos analíticos tradicionais, comumente aplicados em óleos e gorduras, assim como uma técnica inovadora, a espectrometria de massas ambiente com ionização por sonic-spray (EASI-MS). Inicialmente, amostras de biodiesel foram oxidadas e analisadas em diferentes intervalos de tempo empregando métodos tradicionais e a técnica EASI-MS. Dentre os métodos tradicionais, o índice de peróxido, que mede os compostos primários de oxidação, destacou-se como o principal parâmetro que se alterou durante o período de indução (PI) do biodiesel de soja oxidado em Rancimat a 110°C. Apenas a partir do PI, ocorreu efetivamente a formação dos compostos secundários. Esse comportamento foi evidenciado pelo aumento no índice de anisidina, compostos polares, acidez e viscosidade cinemática. A taxa de formação dos compostos de oxidação foi maior à medida que se elevou a temperatura, empregando-se as condições de temperatura ambiente, estufa a 60°C e Rancimat a 110°C. Além disso, o fim da estabilidade do biodiesel de soja em condições de armazenamento foi previsto utilizando uma equação exponencial obtida com os dados de testes acelerados em Rancimat. De acordo com os resultados obtidos com a técnica EASI-MS, foi possível identificar, a nível molecular, compostos secundários de oxidação, tais como os aldeídos e os dímeros. Estes compostos caracterizam amostras em estágios avançados de oxidação. Adicionalmente, a técnica EASI-MS mostrou-se eficiente em avaliar a oxidação do biodiesel de soja e soja/sebo (70/30) durante sua vida útil baseado no monitoramento do íon de m/z 349. Este íon corresponde ao principal hidroperóxido encontrado nessas amostras. Em conclusão, esse trabalho possibilitou verificar os principais parâmetros oxidativos e de qualidade que se alteram durante a oxidação do biodiesel, bem como demonstrou que o EASI-MS é uma ferramenta analítica simples e rápida que pode ser utilizada como uma técnica de screening da qualidade oxidativa do biodiesel / Abstract: The use of biodiesel in the Brazilian's energy matrix presents several technological, environmental, and social advantages. However, note that biodiesel is less stable to storage compared to diesel. In this context, the aim of this work was to study the oxidation behavior of biodiesel using traditional analytical methods normally applied to oils and fats as well as an innovative technique, the Easy Ambient Sonic-spray Ionization Mass Spectrometry (EASI-MS). Initially, biodiesel samples were oxidized and analyzed at different time intervals using traditional methods and EASI-MS. Among the traditional methods, the peroxide value, which measures the primary oxidation products, was the major parameter that changed during the induction period (IP) of soybean biodiesel samples oxidized in Rancimat at 110°C. The formation of the secondary oxidation products occurred primarily after the IP, which was evidenced by the increase in the anisidine value, polar compounds, acidity, and kinematic viscosity. The rate of formation of the oxidation products was higher as the assay temperature increased, using samples at room conditions, oven at 60°C, and Rancimat at 110°C. Additionally, the end of soybean biodiesel stability at room temperature was predicted using an exponential model fitted to data obtained in accelerated oxidation experiments. According to results obtained by EASI-MS, it was possible to identified secondary oxidation products at the molecular level, such as aldehydes and dimers. These products characterize biodiesel samples in advanced stages of oxidation. Additionally, EASI-MS was shown to be efficient to evaluate the oxidation of soybean and soybean/beef tallow (70/30) biodiesel samples during its shelf-life based on the evolution of the ion of m/z 349. This ion corresponds to the major hydroperoxide formed at those biodiesel samples. In conclusion, the main parameters that change during the oxidation of biodiesel were verified in this study. Additionally, it was also demonstrated that EASI-MS is a simple and fast analytical tool able to be used as a screening technique to evaluate the oxidative quality of biodiesel / Doutorado / Tecnologia de Alimentos / Doutor em Tecnologia de Alimentos
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Characterization of chemical compounds in plants by Direct Electrospray probe Mass SpectrometryChan, Tsung-Hsun 01 September 2011 (has links)
Ambient ionization mass spectrometry is a technique used for the analysis of samples under ordinary ambient conditions. It has many advantages, such as fast sample exchange, low operation time and few sample preparation which comparing with thus ion source operating in vacuum. Therefore, several different ambient ionization sources have been developed in the past decade.
Direct Electrospray Probe ionization mass spectrometry (DEP-MS) was developed by Shiea, J in 1999, which providing an effective means of analyzing not only large biomolecules, but also small organic and inorganic compounds. It can rapidly generate electrospray from a droplet which was deposited on a probe. The DEP technique provides a number of unique analytical features containing: (a) low sample consumption and sample switching is immediate; (b) the capillary and pump are unnecessary; and (c) the probe is low-cost and easy to construct and clean, and is free to maintenance.
The first part of experiment in this research is based on the ideal of DEP. The leaf tissues were cut into a triangular shape, 15 mm long and 8 mm wide at the base, is held by a crocodile clip with the apex facing the inlet of the mass spectrometer and at a distance of 2 cm or more from it. Electrospray solutions are added onto the tissue to mix with the leaf sap, and a high voltage (4.5-5.5 kV) is applied to the leaf tissue through the crocodile clip, and generate ions for MS analysis. This method has been demonstrated to be applicable for the analysis of a wide variety of plant sample, such as the leaves tissue in different color, different growth, diseased and pesticide residue.
The second part of experiment is improved from the first research. Electrospray was produced via a metal probe which binding two fine stainless steel needle (0.27 mm diameter) together. This probe plays the role of sampling and ionization. An amount of liquid sample was loaded onto the probe when the tip of probe touched the plant tissue, then electropray solution are introduced by syringe pump into the probe and applied high voltage on the probe to produce electrospray ionization. Therefore, direct rapid analysis was achieved using this probe interfaced and this method can direct profile of phytochemicals in a section of plant tissue in different regions, including root, stem, leaf, outer and inner part of fruit. In addition, using this probe, solid samples are directed sampling equally. The solid materials can be observed on the tip of probe by scanning electron microscope (SEM). It can obtain reasonable strong ion signals rapidly for agrochemicals deposited on the surface of vegetables or fruits peel.
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Ambient Liquid Mass Spectrometry: Development and ApplicationYuan, Cheng-hui 19 July 2007 (has links)
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Analysis of the Compositional Variation in the Epicuticular Wax Layer of Wheat (Triticum aestivum)Beecher, Francis Ward 03 October 2013 (has links)
Epicuticular waxes form a layer on the outer surface of all land plants and play a fundamental role in their interaction with the environment. Development of a rapid and accurate method for the characterization of these waxes could allow the use of wax composition as a novel phenotype during plant breeding and selection. In this study, the suitability of Direct Analysis in Real Time Mass Spectrometry (DART-MS) for the characterization of epicuticular waxes was investigated. This method provides a “fingerprint” of the relative abundance of all constituents in the analyte based on mass, is suitable for very high throughput, requires minimal sample preparation, and is able to provide for the characterization of even complex biological mixtures. Herein, the suitability of DART-MS for analysis of epicuticular wax was investigated through analysis of samples of extracted wax collected from the flag leaves of a 279 line association mapping population grown across four environments with two replicates in both irrigated and drought treatments. Additionally, for a subset of samples, wax was collected from glumes in order to test for differences in wax composition between tissue types. In all, a total of 3,454 wax extracts were analyzed with three technical replicates. The above analysis generated a total of 13,164 mass spectra (“fingerprints”), made at an average rate of 30 seconds each. Multivariate analyses including random forest, principal component analysis, and linear discriminant analysis, were used to identify the presence of differences between the spectra of wax from different tissues (leaves/glumes) and treatment types (irrigated/drought). The peaks best serving as predictors of sample class for each comparison were examined, and tentative identifications were made through comparison of the associated mass with literature and publicly available databases. As a separate test of concept, the ability to distinguish between the epicuticular wax compositions of individual varieties was determined through analysis of a group of closely related lines developed at CIMMYT which differed in agronomic performance.
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Applications of Direct Electrospray Probe Mass Spectrometry in Studying Change of Chemical Compounds in PlantsTsai, Yung-Chi 04 September 2012 (has links)
Ambient mass spectrometry is one of the mainstream techniques in modem mass spectrometry development. The developing purpose of ambient mass spectrometry is improving the analysis efficiency and simplifying operation process. So that, there are many techniques about ambient mass spectrometry had been published and commercialized. And direct electrospray probe mass spectrometry (DEP/MS) is one of ambient mass spectrometry techniques which is emphasized its rapid analysis and high sampling space resolution.
In this research we improved the DEP system for more suitable in rapid analysis. We rule of the use of Syringe pump and its tube. Replace it by using solution tank so that we can save the time cost by disassemble syringe pump and tube when sampling. We also change the electric field by different high voltage applied mode for safety concern.
In this study DEP/MS were used in plants analysis applications: capsaicin in peppers, systematic pesticide absorption in tomato and toxic compounds distribution in potato surface.
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Development and Applications of Laser-Induced Acoustic Desorption/Electrospray Ionization Mass SpectrometryCheng, Sy-Chyi 27 January 2010 (has links)
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Caracterização de lecitinas comerciais por espectrometria de massas ambiente com ionização sonic-spray / Characterization of commercial lecithins by easy ambient sonic-spray ionization mass spectrometryFernandes, Gabriel Deschamps, 1988- 19 August 2018 (has links)
Orientador: Daniel Barrera Arellano / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-19T21:15:47Z (GMT). No. of bitstreams: 1
Fernandes_GabrielDeschamps_M.pdf: 1854677 bytes, checksum: e57833484e8f9ad4a136187bed59d8d2 (MD5)
Previous issue date: 2012 / Resumo: Os fosfolipídios são definidos como o grupo de moléculas que contém um grupamento fosfato. Por apresentarem características anfipáticas, este grupo de moléculas se organiza naturalmente em bicamadas, originando as membranas dos seres vivos. Industrialmente são capazes de estabelecer interfaces óleo/água, possibilitando a formação e estabilização de emulsões. Este grupo de moléculas é bastante diverso quimicamente, sendo os principais componentes a fosfatidilcolina, fosfatidiletanolamina, fosfatidilserina, fosfatidilinositol, ácido fosfatídico e esfingomielina. A determinação e quantificação desses compostos é bastante laboriosa tanto nos meios industriais como acadêmicos, envolvendo, entre outras, etapas de digestão ácida e incineração. A espectrometria de massas desponta como uma técnica bastante favorável à análise de lipídios, englobando desde estudos clínicos até de biocombustíveis. Mais recentemente, as técnicas de espectrometria de massas com ionização ambiente facilitaram o acesso a este tipo de tecnologia, diminuindo os custos de implantação e principalmente de operação. A ionização ambiente por sonic-spray (EASI, easy ambient sonic-spray ionization) denota-se como uma técnica adequada à análise de lipídios, uma vez que não aplica alta voltagem e alta temperatura, prevenindo, portanto possíveis degradações destas moléculas. Este trabalho teve como objetivo, estudar a ionização de fosfolipídios (PL) e triacilgliceróis (TAG) frente à técnica EASI-MS, bem como, estudar a viabilidade técnica da caracterização de lecitinas comerciais por meio da técnica EASI-MS. Quanto à ionização dos lipídios, foi possível observar, nas condições de estudo, que dentro de uma mesma classe (PL ou TAG) a intensidade de ionização diminui com o aumento da cadeia dos ácidos graxos e aumenta com o aumento das insaturações. Para o estudo de caracterização foram utilizadas seis amostras de lecitina de soja comercial, obtidas por diferentes processos. As amostras foram diluídas em clorofórmio e submetidas à análise de EASI-MS, nos modos positivo e negativo. Nos espectros de EASI(+)-MS, os íons mais representativos foram os íons correspondentes à fosfatidilcolina e aos triacilgliceróis, enquanto que, nos espectros de EASI(-)-MS os íons mais representativos corresponderam à fosfatidiletanolamina, aos ácidos graxos livres e aos glicofosfolipídios. A técnica EASI-MS mostrou-se eficiente na caracterização das lecitinas comerciais. Sendo uma técnica rápida e que não exige preparo de amostra / Abstract: Phospholipids are defined as the group of molecules containing a phosphate grouping. As they have amphipathic characteristics, this group of molecules naturally organizes bilayer, origin the membranes of living organism and are able to establish an industrial oil / water interface, allowing the formation and stabilization of emulsions. This group of molecules is very chemically different; the main components are phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylinositol, phosphatidic acid and sphingomyelin. The determination and quantification of these compounds is very laborious for the academic and industrial circles, involving, among others, several steps, like acid digestion and incineration. Mass spectrometry is emerging as a very favorable tool of lipids analysis, since clinical and biofuel studies. Recently, the techniques of ambient mass spectrometry have facilitated the access to this type of technology, reducing deployment costs and especially the operation. Easy ambient sonic-spray ionization (EASI) denotes as a suitable technique to analyze the lipids, since it does not apply high voltage and high temperature, and thereby prevent possible degradation of these molecules. This work aimed to study the ionization of phospholipids (PL) and triacylglycerols (TAG) in EASIMS technique, as well as studying the technical feasibility of the characterization of commercial lecithins by EASI-MS. On the lipid ionization, it was observed, under the conditions of the study, that within the same class (TAG or PL) the ionization intensity decreases with increasing of fatty acids chains and increases with increasing of unsaturation. For characterization studies were used six samples of commercial soy lecithin, obtained by different processes. Samples were diluted in chloroform and analyzed for EASI-MS in positive and negative ion modes. In the spectra of EASI (+)- MS, the most representing ions are corresponding to triglycerides and phosphatidylcholine, whereas in the spectra of EASI (-)-MS the most representative ions correspond to the phosphatidylethanolamine, the free fatty acids and glicophospholipidios. The EASI-MS technique was efficient in the characterization of commercial lecithins. As a fast technique and does not require sample preparation / Mestrado / Tecnologia de Alimentos / Mestre em Tecnologia de Alimentos
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