Background: Vincetoxicum iphisia Meve and Liede is a lesser-known medicinal plant species with limited phytochemical characterization despite its traditional uses. This study aimed to investigate the bioactive metabolite profile of ethanol extracts from the bark and leaves of V. iphisia using Liquid Chromatography-Mass Spectrometry (LC-MS). Materials and Methods: Ethanol extracts were prepared from the bark and leaves and analyzed using LC-MS. Metabolites were identified based on retention time, molecular weight, and database comparisons. Total Ion Chromatograms (TICs) and Base Peak Intensity (BPI) profiles were used to assess shared and tissue-specific compounds. Results: LC-MS profiling revealed a range of pharmacologically relevant secondary metabolites including flavonoids (e.g., quercetin, isorhamnetin derivatives), phenolic glycosides, coumarins, alkaloids (e.g., L-kynurenine), and linear diarylheptanoids. Key compounds such as cinobufagin, catechin gallate, and triptophenolide known for their antioxidant, anti-inflammatory, cardioprotective, and anticancer effects were identified. Conclusion: This first LC-MS-based investigation of V. iphisia highlights its rich metabolite diversity and supports its potential as a source of pharmacologically important natural products, warranting further biological and mechanistic studies.