In situ highly sensitive potential- and time-resolved monitoring of polycrystalline gold and platinum electrochemical dissolution in pure organic media is reported. This was achieved by successfully upgrading electrochemical flow cell coupled to inductively coupled plasma mass spectrometry. Similar to the aqueous media, aggressive transient dissolution takes place during oxide formation and reduction. In contrary to the aqueous electrolyte, both gold and platinum exhibit enhanced anodic compared to the cathodic oxide-assisted dissolution in organic media. This study intends to highlight the capabilities of the new methodology, which will expand the studies of metals dissolution to the fields like organic electrocatalysis, corrosion, battery research, and sensors among others.