Alkaloids of the aerial parts of P. multisectum (Maxim) Bobrov (Zygophyllaceae) growing in Mongolia have been studied by capillary Gas Chromatography-Mass Spectrometry (GC-MS) and Column Chromatography (CC). Four compounds comprising of 2-methylquinoline (1), 9-amino-2, 3,5,6,7,8-hexahydro-1H-cyclopenta [b] quinoline (2), vasicinone (3) and harmine (4) have been determined by GC-MS, while harmine (4), peganine (5), deoxypeganine (6), deoxyvasicinone (7) and harmane (8) were isolated as pure compounds by the CC. The structures of the five alkaloids 4, 5, 6, 7 and 8 were elucidated by the MS and 1H and 13C NMR analysis. The alkaloids 1, 2 and 8 were identified for the first time from this species.Mongolian Journal of Chemistry 16 (42), 2015, 48-53