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There is widespread use of ionization sources (ambient and non-ambient) for a variety of applications. More recently, charged microdroplets generated by electrospray ionization and paper spray have been used to conduct chemistry at faster rates compared to bulk volumes. Uncharged droplets such as those generated by the Leidenfrost technique have also been used to explore chemistry and study the degradation of drugs in an accelerated manner. These microdroplets serve as reaction vessels in which in which some reactions are known to occur at accelerated rates. Such chemistry can be particularly useful in pharmaceutical settings to rapidly synthesize small amounts of materials in relatively short amount of time. Additionally, microdroplets may also be used to perform high throughput screening analysis. While several parameters influencing the rate of reaction in microdroplets have been explored (such as spray distance and reagent concentration), the mechanism of reaction acceleration has not been probed to a significant extent. A major portion of my dissertation describes the use of charged and uncharged microdroplets to perform quick chemistry, guide microfluidic synthesis of drugs such as diazepam, perform scale up of copper catalyzed C-O and C-N coupling reactio<a></a>ns and screen reaction conditions for pharmaceutically relevant reactions such as the Suzuki cross-coupling reaction. Additionally, work discussed here also describes development and use of existing techniques such as structured illumination microscopy to measure droplet sizes, explore the role of distances on droplet size, and study the effect of surfactants on the rate of reactions in microdroplets generated by nano-electrospray ionization. A mathematical model to understand the mechanism of increased reaction rates in microdroplets has also been presented. Additionally, this dissertation also describes ways to manipulate ions in air using various designs of 3D-printed electrodes that operate with DC potentials only and which can be easily coupled with nano-electrospray ionization sources to transmit ions over long distances

<p dir="ltr">Mass spectrometry (MS) is a comprehensive and adaptable technique that is useful for addressing a wide range of complex analytical challenges. In this work MS-based assays were developed to address issues relating to the synthetic drug epidemic and failures in point-of-care situations. Chapter one is an overview of the history of mass spectrometry, the fundamental operation of a mass spectrometer, and the advancements made in ionization methods. Chapter two is a review focusing on drug surveillance programs, or lack thereof, and their impact on combating the synthetic drug epidemic in the United States. The work in chapter three describes the development of a novel untargeted semiquantitative paper spray mass spectrometry assay for synthetic drug screening in human plasma. This work implemented a 3D printed solid phase extraction cartridge that allowed for sample preconcentration. This method was tested using remnant patient plasma samples collected from local downtown Indianapolis hospitals. Chapter four introduces a comparison of mass spectrometry acquisition methods to determine the most sensitive and specific techniques. The acquisitions that are compared are parallel reaction monitoring (PRM), sequential windowed acquisition of all theoretical mass (SWATH), and data dependent acquisition (DDA). A small subset of synthetic drugs with known properties were chosen for this comparison and a confirmation study was conducted with real patient samples. Chapter five details a combined approach for the determination of methylpyridine derivative isomers utilizing gas chromatography infrared spectroscopy (GC-IR), gas chromatography mass spectrometry (GC-MS), and density functional theory (DFT) calculations. The projects detailed herein show the extensive range with which mass spectrometry can be used for the detection of a wide range of drugs and synthetic compounds.</p>

<p dir="ltr">Laser-induced acoustic desorption (LIAD) is an evaporation technique that allows for thermally labile, nonvolatile neutral compounds to be vaporized without the need for derivatization or excessive heating. After a thin coating of a sample is applied to a titanium foil, the opposite side of the foil is subjected to laser irradiation to desorb neutral compounds from the opposite side into the gas phase. LIAD shows great potential for facilitating the analysis of a wide variety of compounds when coupled with molecular rotational resonance (MRR) spectroscopy. In this work, a few model compounds were chosen based on previous research to optimize the sample preparation and foil deposition methods for LIAD/MRR spectroscopy. One possible strategy to maximize the MRR signal is attempting to generate amorphous samples on the foils instead of ordered, crystalline samples. Changing the solvents used for dissolution of the compounds and freeze-drying the sample before deposition were also investigated.</p>

<p>U okviru disertacije ispitani su i upoređeni pokazatelji kvaliteta integralnog p&scaron;eničnog i integralnog heljdinog bra&scaron;na dobijenog mlevenjem netretiranih (netretirano integralno heljdino bra&scaron;no) i autoklaviranih zrna heljde (autoklavirano integralno heljdino bra&scaron;no). Nakon ispitivanja nutritivnih i funkcionalnih svojstava pomenutih bra&scaron;na, kreirane su i proizvedene integralne taljatele sa različitim sadržajem integralnog heljdinog bra&scaron;na (10&ndash;30%).<br />Pokazatelji senzorskog, nutritivnog i funkcionalnog kvaliteta proizvedenih taljatela sa integralnim heljdinim bra&scaron;nima ispitani su u poređenju sa kontrolnim uzorkom taljatela od integralnog p&scaron;eničnog bra&scaron;na.<br />U ispitivanim uzorcima bra&scaron;na i taljatela određeni su osnovni hemijski sastav, sadržaj mineralnih materija, sadržaj ukupnih rastvorljivih polifenola, utvrđen je kvalitativni i kvantitativni sastav polifenolnih jedinjenja, ispitana je antiradikalska aktivnost na DPPH˙ i određen je sadržaj fitinske kiseline i 5-hidroksimetilfurfural.<br />Pored analize nutritivnih i funkcionalnih svojstava, na taljatelama su sprovedena ispitivanja fizičkih osobina (dimenzije) i svojstva taljatela pri kuvanju. Instrumentalno su izmereni boja i teksturna svojstva nekuvanih i kuvanih taljatela. Senzorska ocena taljatela sprovedena je uz primenu panela utreniranih ocenjivača, metodom bodovanja i panela potro&scaron;ača, testom dopadljivosti.<br />Dobijeni rezultati ukazuju da se supstitucijom dela integralnog p&scaron;eničnog bra&scaron;na integralnim heljdinim bra&scaron;nom (autoklaviranim ili netretiranim) postiže unapređenje nutritivnog i funkcionalnog profila uzoraka obogaćenih taljatela, uz manje ili vi&scaron;e izraženo naru&scaron;avanje senzorskog profila, u zavisnosti od stepena supstitucije i vrste integralnog heljdinog bra&scaron;na.</p> / <p>This study investigated quality parameters of wholegrain wheat flour and wholegrain buckwheat flour from non-treated buckwheat grains (non-treated wholegrain buckwheat flour) and autoclaved buckwheat grains (autoclaved wholegrain buckwheat flour). After investigation of nutritional and functional properties of aforementioned flours, new wholegrain tagliatelle formulations, with different wholegrain buckwheat flour content (10&ndash;30%) have been developed.<br />Sensory, nutritional and functional quality parameters of buckwheat containing tagliatelle samples were analysed and compared with control tagliatelle sample from wholegrain wheat flour.<br />Proximate composition, content of minerals, content of total polyphenols and quantitative and qualitative composition of polyphenols were investigated in both, flour samples and produced uncooked and cooked tagliatelle samples. Antiradical activity on DPPH radicals, and content of less favourable compounds, phytic acid and HMF, have been tested, as well.<br />Tagliatelle physical properties, dimensions, cooking properties, colour and textural properties were determined by instrumental and sensory methods. Tagliatelle acceptability was evaluated by the consumers. The obtained results indicate that wholegrain buckwheat flour (autoclaved or non-treated) incorporation into tagliatelle formulation led to an improvement of nutritional and functional profiles of tagliatelle samples, followed by greater or lesser deterioaration of sensory profile, depending on substitution level and type of wholegrain buckwheat flour.</p>

<p>Сензорска анализа представља јединствено средство за праћење органолептичких својстава хране уз примјену људских чула, јер је најближа потрошачкој оцјени и уједно веома поуздан тест у пружању свеобухвтане оцјене квалитета прехрамбеног производа. Она представља најважнију референцу наспрам резултата добијених хемијским или инструменталним методима и њиховим поређењем омогућује прихватање, одабир или побољшање било којег другог метода.<br />Имајући у виду сву комплексност текстурних својстава тјестенине, као и важност објективизације појединих њених сегмената у циљу задовољења тржишта, праћења производње и задовољења важећих одредби правилника и прописа, у овом раду спроведена је објективна сензорска оцјена одабраних текстурних својстава тјестенине, као и њихова оцјена примјеном инструменталних метода.<br />Испитивања су спроведена на комерцијалним узорцима сушене тјестенине облика шпагете, поријеклом од домаћих и страних произвођача, најчешће присутних у већим тржним центрима наше земље. Поред анализе хемијског састава и својстава при кувању, на формираном сету узорака шпагета спроведена су испитивања одабраних текстурних својстава сушених и куваних облика примјеном сензорске оцјене и инструменталних одређивања.<br />Упркос добрим слагањима резултата добијених инструменталних одређивањим и сензорском оцјеном од стране панела одабраних оцјењивача, дошло се до закључка да поједини инструментални методи могу наћи добру примјену у предикцији објективне сензорске оцјене појединих текстурних својстава и тиме допринијети побољшању квалитета тјестенине облика шпагета током технолошког процеса производње, али да не могу безрезервно бити прихваћени као алтернатива објективној сензорској оцјени у предикцији потрошачке прихватљивости овог прехрамбеног производа на тржишту.</p> / <p>Senzorska analiza predstavlja jedinstveno sredstvo za praćenje organoleptičkih svojstava hrane uz primjenu ljudskih čula, jer je najbliža potrošačkoj ocjeni i ujedno veoma pouzdan test u pružanju sveobuhvtane ocjene kvaliteta prehrambenog proizvoda. Ona predstavlja najvažniju referencu naspram rezultata dobijenih hemijskim ili instrumentalnim metodima i njihovim poređenjem omogućuje prihvatanje, odabir ili poboljšanje bilo kojeg drugog metoda.<br />Imajući u vidu svu kompleksnost teksturnih svojstava tjestenine, kao i važnost objektivizacije pojedinih njenih segmenata u cilju zadovoljenja tržišta, praćenja proizvodnje i zadovoljenja važećih odredbi pravilnika i propisa, u ovom radu sprovedena je objektivna senzorska ocjena odabranih teksturnih svojstava tjestenine, kao i njihova ocjena primjenom instrumentalnih metoda.<br />Ispitivanja su sprovedena na komercijalnim uzorcima sušene tjestenine oblika špagete, porijeklom od domaćih i stranih proizvođača, najčešće prisutnih u većim tržnim centrima naše zemlje. Pored analize hemijskog sastava i svojstava pri kuvanju, na formiranom setu uzoraka špageta sprovedena su ispitivanja odabranih teksturnih svojstava sušenih i kuvanih oblika primjenom senzorske ocjene i instrumentalnih određivanja.<br />Uprkos dobrim slaganjima rezultata dobijenih instrumentalnih određivanjim i senzorskom ocjenom od strane panela odabranih ocjenjivača, došlo se do zaključka da pojedini instrumentalni metodi mogu naći dobru primjenu u predikciji objektivne senzorske ocjene pojedinih teksturnih svojstava i time doprinijeti poboljšanju kvaliteta tjestenine oblika špageta tokom tehnološkog procesa proizvodnje, ali da ne mogu bezrezervno biti prihvaćeni kao alternativa objektivnoj senzorskoj ocjeni u predikciji potrošačke prihvatljivosti ovog prehrambenog proizvoda na tržištu.</p> / <p>Sensory analysis represents the unique tool for determination of organoleptic properties of food using human senses, because it is highly correlated with the consumers&rsquo; opinion. At the same time it is very reliable test for obtaining the comprehensive evaluation of foodstuffs quality. Moreover, the sensory analysis is the most important reference versus the results of chemical or instrumental methods, and their comparison enables adoption of any other method used for determination of sensory properties. Bearing in mind the complexity of the textural properties of pasta and the significance of objectivity of its methodology, this thesis conducted the objective evaluation of selected sensory textural properties of pasta and their evaluation by the instrumental methods as well. Nine commercial spaghetti samples produced by foreign and domestic producers were chosen for the study. The selected textural properties of dry and cooked spaghetti determined by sensory and instrumental methods comprised shape. The obtain results showed that applied instrumental methods provided reliable prediction of the objective sensory evaluation of certain spaghetti textural properties. Thus, their use may contribute to the improvement of spaghetti quality during production process. Despite the good agreement between the results obtained by instrumental and sensory methods, the instrumental methods could not be unconditionally accepted as the alternative to sensory evaluation in predicting consumers&rsquo; acceptance of spaghetti on the market.</p>

O presente trabalho aborda a interação entre a utilização do Méthode pour la Guitare (1830) de Fernando Sor com o processo de construção de interpretação da Sonata op. 25, do mesmo autor. O trabalho foi norteado pela hipótese de associação entre as concepções técnicas e composicionais de Sor, articuladas em seu Método, e sua correspondente tradução em sua escrita violonística. Através desse cotejo, traçaram-se claras possibilidades de associação, e concluiu-se positivamente na utilização do Método como ferramenta complementar na interpretação da música de Fernando Sor. / The present work concerns the interaction between the use of the Méthode pour la guitare (1830) by Fernando Sor and the process of constructing an interpretation for the Sonata op. 25, by the same author. The work‟s main hypothesis was the association between technical and compositional conceptions of Sor, displayed in his Method, and their correspondent translation into his guitar compositional writing. Through this association, clear relationships were established and the work was conclusive on the positive use of the Method as a complementary tool for the interpretation of Fernando Sor‟s music. / El presente trabajo aborda la interacción entre la utilización del Méthode pour la guitare (1830) de Fernando Sor con el proceso de construcción de una interpretación para la Sonata op. 25, del mismo autor. La hipótesis del trabajo fue la asociación entre las concepciones técnicas y compositivas de Sor, articuladas en su Método, y su correspondiente traducción en su escritura guitarrística. Por medio de este cotejo, se trazaron claras posibilidades de asociación, y se concluyó positivamente por el uso del Método como herramienta complementaria en la interpretación de la música de Fernando Sor.

O presente trabalho aborda a interação entre a utilização do Méthode pour la Guitare (1830) de Fernando Sor com o processo de construção de interpretação da Sonata op. 25, do mesmo autor. O trabalho foi norteado pela hipótese de associação entre as concepções técnicas e composicionais de Sor, articuladas em seu Método, e sua correspondente tradução em sua escrita violonística. Através desse cotejo, traçaram-se claras possibilidades de associação, e concluiu-se positivamente na utilização do Método como ferramenta complementar na interpretação da música de Fernando Sor. / The present work concerns the interaction between the use of the Méthode pour la guitare (1830) by Fernando Sor and the process of constructing an interpretation for the Sonata op. 25, by the same author. The work‟s main hypothesis was the association between technical and compositional conceptions of Sor, displayed in his Method, and their correspondent translation into his guitar compositional writing. Through this association, clear relationships were established and the work was conclusive on the positive use of the Method as a complementary tool for the interpretation of Fernando Sor‟s music. / El presente trabajo aborda la interacción entre la utilización del Méthode pour la guitare (1830) de Fernando Sor con el proceso de construcción de una interpretación para la Sonata op. 25, del mismo autor. La hipótesis del trabajo fue la asociación entre las concepciones técnicas y compositivas de Sor, articuladas en su Método, y su correspondiente traducción en su escritura guitarrística. Por medio de este cotejo, se trazaron claras posibilidades de asociación, y se concluyó positivamente por el uso del Método como herramienta complementaria en la interpretación de la música de Fernando Sor.

O presente trabalho aborda a interação entre a utilização do Méthode pour la Guitare (1830) de Fernando Sor com o processo de construção de interpretação da Sonata op. 25, do mesmo autor. O trabalho foi norteado pela hipótese de associação entre as concepções técnicas e composicionais de Sor, articuladas em seu Método, e sua correspondente tradução em sua escrita violonística. Através desse cotejo, traçaram-se claras possibilidades de associação, e concluiu-se positivamente na utilização do Método como ferramenta complementar na interpretação da música de Fernando Sor. / The present work concerns the interaction between the use of the Méthode pour la guitare (1830) by Fernando Sor and the process of constructing an interpretation for the Sonata op. 25, by the same author. The work‟s main hypothesis was the association between technical and compositional conceptions of Sor, displayed in his Method, and their correspondent translation into his guitar compositional writing. Through this association, clear relationships were established and the work was conclusive on the positive use of the Method as a complementary tool for the interpretation of Fernando Sor‟s music. / El presente trabajo aborda la interacción entre la utilización del Méthode pour la guitare (1830) de Fernando Sor con el proceso de construcción de una interpretación para la Sonata op. 25, del mismo autor. La hipótesis del trabajo fue la asociación entre las concepciones técnicas y compositivas de Sor, articuladas en su Método, y su correspondiente traducción en su escritura guitarrística. Por medio de este cotejo, se trazaron claras posibilidades de asociación, y se concluyó positivamente por el uso del Método como herramienta complementaria en la interpretación de la música de Fernando Sor.