In this chapter, we describe volatile and nonvolatile metabolite identification methods in durian pulp using gas chromatography-mass spectrometry (GC-MS). Special focus is given to sulfur-containing volatile compounds, such as methanethiol, ethanethiol, and hydrogen sulfide, as well as key metabolites that contribute to the characteristic aroma of durian. In addition, we detail the methodologies for metabolite extraction, chemical derivatization, and identification of primary metabolites, including sugars, amino acids, and organic acids. Moreover, we provide a collection of durian samples and highlight the importance of defining maturity and ripening stages, as these factors influence metabolite composition. The methods described in this chapter could serve as a model for studying metabolite profiling in other fruits, with potential applications in food science and agricultural research.