The use of hyphenated LC-NMR and LC-MS techniques for the purpose of directly identifying the major constituents of Belamcanda chinensis was investigated. Reversed-phase isocratic chromatography was performed using an acetonitrile-water solvent system on a C18 column. The NMR spectrum yielded five main peaks, whose analysis revealed them to be 5, 6, 7, 3'-tetrahydroxy-4'-methoxyisoflavone (1), tectorigenin (2), iristectorigenin A (3), irigenin (4), and irisflorentine (5). The identification of these constituents was confirmed by performing LC-ESI-MS experiment. This study shows that hyphenated LC-NMR and LC-MS can be used for the rapid (70 min) identification of the isoflavonoids.