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This dissertation delves into the contemporary significance of carbohydrates across diverse life forms and industries, emphasizing their pivotal role in shaping product quality, safety, and regulatory compliance within sectors like food and beverage, pharmaceuticals, and biofuels. The research capitalizes on significant advancements in nuclear magnetic resonance (NMR) spectroscopy, specifically silicon-29 NMR, extending its applications beyond protons to exert influence in fields such as materials science, biochemistry, and environmental science. A focal point of the study involves the synthesis of twelve per-O-silylated sugars using a microwave reactor, strategically reducing reaction time while preserving yield. Advanced NMR experiments identify silicon signals, providing valuable insights into spatial orientation and distinctive structural variations. The analysis of chemical shifts in per-O-silylated sugars contributes to the establishment of an extensive silicon NMR database for comprehensive carbohydrate characterization. Noteworthy patterns in per-O-silylated sugars, along with the discernible chemical shifts in diverse silylated compounds, further enhance the depth of the database. Recent strides in the 29Si NMR characterization technique are underscored, with a specific focus on per-O-silylated sugars. The characterization of twelve per-silylated sugars using 29Si NMR spectroscopy, complemented by a 2D graph incorporating 13C NMR chemical shifts, introduces an innovative approach that optimizes visualization and streamlines compound identification. Despite encountering challenges in a mixture synthesis experiment, where silicon chemical shifts undergo slight changes, the study contributes significantly to our understanding of per-O-silylated sugars using 29Si NMR spectroscopy. The dissertation concludes by addressing the limitations of 1H NMR spectroscopy, introducing the prominence of 1H quantitative nuclear magnetic resonance (qNMR). The Gervay-Hague research group employs 29Si NMR spectroscopy to quantify glucose, sucrose, and fructose within mixtures, which could extend the analysis to encompass coffee and tea leaves. Insights derived from 29Si NMR analysis affirm the reliability of integrated resonances, with the incorporation of a novel internal standard leading to a notable reduction in errors. The 29Si NMR signal corresponding to the 2-hydroxyl position emerges as a consistent and promising diagnostic tool for the quantitative assessment of sample mixtures, thereby showcasing the potential for accurate carbohydrate measurement across a spectrum of applications.