Presented is a solid-phase microextraction syringe-electrode assembly that may be used to identify electrode reaction products. After an electrochemical experiment, the electrode within this syringe-electrode assembly can be introduced into the injection port of a gas chromatograph. Electrochemical reaction products can be analyzed, provided they adhere to the electrode surface and are amenable to gas chromatographic/mass spectrometric analysis. We highlight the potential usefulness of this device using well-known electrochemical reaction of quinones.