From the whole plants of Macrosolen tricolor, three phenolics, gallic acid (1), 3,3'-di-O-methylellagic acid (2), 3,3'-di-O-methylellagic acid 4-O--D-xylopyranoside (3), three flavonoids, kaempferol (4), vitexin (5), orientin (6), and two steroids, stigmast-5-ene 3-O--D-glucopyranoside (7), and stigmast-5-ene 3-O--D-(6'-Omargaroyl)glucopyranoside (8) were separated. Their chemical structures were illuminated by HRMS, and NMR as well as comparison with those data. Compound 6 was first reported from M. tricolor and compounds 1-5, 7, and 8 were first isolated from genus Macrosolen.