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The plant kingdom is still an untapped reservoir of new molecules with therapeutic potential. A selection of bioactive plant constituents recently discovered are presented with focus on new drugs or lead compounds in an advanced state of development. Obtaining pure new biologically active substances from plants remains a complex task. Biological and chemical screenings are complementary approaches for the rapid detection and isolation of new interesting plant constituents. Biological screening followed by activity-guided fractionation has been successfully used in our laboratories for the discovery of new antifungal metabolites and inhibitors of enzymes involved in the aetiology of prostate hyperplasia. High-performance liquid chromatography (HPLC) coupled to UV spectroscopy (LC/UV), mass spectrometry (LC/MS), and magnetic resonance (LC/NMR) proved to be highly efficient for the chemical screening of crude plant extracts. These hyphenated techniques were extensively used for the investigation of polyphenols with monoamine-oxidase inhibitory (IMAO) properties in Gentianaceae species.