The determination of nitrite content in drinking water, smoked bamboo shoot, grandmother food and roasted ear tip was studied by using headspace-gas chromatography, and a fast, accurate and quantitative detection method of nitrite was established. The reaction mechanism of this method was deduced, and the relative products were validated by the headspace gas chromatography-mass spectrometry. The sample solution of smoked bamboo shoot, grandmother food and roasted ear tip were analyzed after crushing, boiling water extraction, precipitation and filtration, and then sodium cyclamate and sulfuric acid solution were added to pretreated sample. Diazo reaction was reacted in headspace bottle at 50 ℃, using the derivatives of cyclohexene as the target product and quantitative analysis. In this paper, the low concentration standard material standard curve r² was 0.999 0. Moreover, the corresponding detection range was 0.001 ~ 0.200 mg/L when 5 mL sample was used. However, the high concentration standard material standard curve r² was 0.999 5, and the corresponding detection range was 0.67~167.00 mg/kg while was 3 g sample was used. It was verified to be a good method for the detection of nitrite in food, with low detection limit, wide linear range, and good repeatability and recovery rate.