We report here an easily applicable method for the quantification of nitrite (NO2−) in real samples. This approach simplified the two steps of sample preparation and detection into a 2‐in‐1 single step process. Samples were digested in sulfuric acid and the as‐generated nitric oxide (NO) was detected by an electrochemical sensor in the gas phase. It eliminated almost all of the interferents in the solution phase and hence resulted in a highly selective determination of nitrite suitable for food samples with complicated matrix. We successfully demonstrated the determination of nitrite in sausage and vegetables and further validated the results with an AOAC official reference method.
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