This chapter describes the methodologies employed to identify volatile metabolites in jasmine rice seedling leaf tea processed via freeze-drying or sun-drying, using headspace gas chromatography–mass spectrometry. The profiling focuses on key classes of volatile compounds, including aldehydes, hydrocarbons, alcohols, ketones, carboxylic acids, and other miscellaneous constituents. Among these, 2-methylbutanal, dodecane, 2-ethylfuran, and methylpyrazine were identified as major contributors to the tea’s characteristic aroma, potentially enhancing its sensory appeal. The chapter further details protocols for metabolite extraction, compound identification, data analysis, quality control, and experimental replication. These analytical approaches may serve as a model for metabolite profiling in other herbal teas, with broader applications in functional beverage development and plant-based product innovation.