Abstract: Atmospheric Pressure Photoionization-Mass Spectrometry (APPI-MS) and High Performance Liquid Chromatography (HPLC) are the two analytical methods that were used to characterize Triacylglycerols (TAGs) during flaxseed development. The HPLC method of the oils showed the presence of 15 TAG species. In contrast to the HPLC chromatograms, the APPI-MS showed 17 peaks of TAG. APPI-MS is more rapid than the HPLC method (11 min). The iodine value of the oils showed a gradual increase, while the oil stability continuously decreased.