New monomeric Naphthyl-iso-quinoline alkaloids, Yaoundamine A and Ancistrocline were isolated and identified from Ancistrocladus heyneanus stem using HPLC/MS and NMR. Owing to the complexity of the extracts, the application of reverse phase HPLC resulted in a partially incomplete separation of the Naphthyl-iso-quinoline alkaloids. By performing HPLC/MS experiments, in combination of parallel isolation studies and structural elucidation using conventional methods, two alkaloids present in the plant could be identified. A. heyneanus stem were collected from the forests of a deep valley of Matheran, Mumbai in Maharashtra, India