<p><i>Ptychopetalum olacoides</i> is a folk medicinal plant for health care in market, especially in Brazil. Fourteen known compounds were isolated from <i>P. olacoides</i> and their chemical structures were elucidated by extensive spectroscopic data, including 1D NMR, 2D NMR, UV, IR and HR-ESI-MS. The 14 known compounds were identified as N-trans-feruloyl-3,5-dihydroxyindolin-2-one (<b>1</b>), magnoflorine (<b>2</b>), menisperine (<b>3</b>), 4-coumaroylserotonin (<b>4</b>), moschamine (<b>5)</b>, luteolin (<b>6</b>), 4′-methoxyluteolin (<b>7</b>), 3-methoxyluteolin (<b>8</b>), 3, 7-dimethoxyluteolin (<b>9</b>), caffeic acid (<b>10</b>), ferulic acid (<b>11</b>), vanillic acid (<b>12)</b>, syringic acid (<b>13</b>) and ginsenoside Re (<b>14</b>). To our knowledge, compounds (<b>1</b>–<b>6</b>, <b>13</b>–<b>14</b>) were isolated from the plant for the first time. Additionally, quantitative analysis results indicated that calibration equations of compounds (<b>1</b>–<b>3</b>, <b>6</b>, <b>9</b>, <b>11</b>–<b>13</b>) exhibited good linear regressions within the test ranges (<i>R</i><sup>2</sup> ≥ 0.9990) and magnoflorine and menisperine were the major constituents in the barks of <i>P. olacoides</i>. The contents of magnoflorine and menisperine accounted for 75.96% of all analytes. However, the content of phenolic components was smaller and the highest content was no more than 1.04 mg/g. Collectively, these results suggested that alkaloids are the dominant substances in <i>P. olacoides</i>, which can make a difference for the quality control and further use of <i>P. olacoides.</i></p
