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Macamides are characteristically found in maca (Lepidium meyenii Walper). Fatty acid derivatives are also an important type of constituent in maca, since they not only relate to the biosynthesis of macamides in the postharvest process but also possess some bioactivities. To study their comprehensive profiles in maca tubers processed via the air-drying method, ultraperformance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) analyses were performed to identify macamide and fatty acid molecules. Their contents in maca tubers that were processed via air drying and freeze drying, respectively, were further quantified using high-performance liquid chromatography (HPLC) analyses comparing with eight macamide and three fatty acid reference standards. A total of 19 macamides (including four novel ones) and 16 fatty acid derivatives (two found in maca for the first time) were identified. Quantification analyses results showed the eight macamides with contents ranging from 31.39 to 1163.19 μg/g (on dry tuber), and fatty acids from 18.71 to 181.99 μg/g in the air-dried maca, but there were only three macamides and one fatty acid detected with very low contents (3.97–34.36 μg/g) in the freeze-dried maca. The results demonstrated that the air-drying method can increase the accumulations of macamides and fatty acids in the metabolism of maca in the postharvest process. The biosynthesis of two types of macamides, i.e., N-benzyl-oxo-octadecadienamides and N-benzyl-oxo-octadecatrienamides, was further elucidated in detail. These results provide more valuable insights into the phytochemicals of maca, which is helpful to explain its health benefits.

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