The nitrite ion (NO2
–) is
used as
a preservative of food and drink and has been widely used in the food
industry. Nonetheless, it is a potential precursor of nitrosamines,
which are known for their carcinogenic activity. Therefore, monitoring
of nitrite in foods and drinks is of paramount importance for food
safety. Herein, we report a very sensitive electroanalytical method
for the determination of nitrite in food samples, capable of detecting
nitrite at the nanomolar level. For that purpose, a nanocomposite
electrode comprising a multilayered film of iron oxide nanoparticles
and reduced graphene oxide (ION-RGO) was decorated with electrodeposited
gold nanoparticles (AuNP) and operated by electrochemical impedance
spectroscopy (EIS). It is observed a synergistic combination of the
electrocatalytic activity of ION-RGO, the electrical conductivity
of AuNP, and the interrogation of the electrode within the charge-transfer
frequency range, which mitigates unwanted capacitive effects and enhances
the nitrite electrooxidation. Consequently, nitrite has been detected
within a wide linear range (r
2 > 0.999)
of 0.58–3019 μM and with a limit of detection of 2.4
nM. Owing to the improved adhesion of AuNP to the ION-RGO framework,
the electrode is highly stable and lasts for at least 30 consecutive
runs without losing its sensitivity. Additionally, the proposed method
enables the determination of nitrite in sausage and milk samples,
when it performs identically to a reference method at the 95% confidence
level.