A method devised for the determination of N-nitrososarcosine, in which the N-nitrosamine in solution is denitrosated with hydrogen bromide to form volatile products that are rapidly removed and determined in a chemiluminescence analyser, has been applied successfully to the same compound on powdered corn flakes. Differentiation of N-nitrososarcosine and a number of other N-nitrosamines and N-nitrosamides from inorganic nitrite was achieved by decomposing the nitrite with acetic acid prior to the denitrosation of the N-nitroso compounds. In the presence of a secondary-amine receptor limited nitrosation can occur during the process of differentiation but this can be prevented through the use of ascorbyl palmitate. In differentiating between large amounts of nitrite and much lower levels of N-nitrososarcosine on corn flakes, using a chemiluminescence analyser, the duration of the response from the nitrite can be shortened by freeze-drying the food matrix in the presence of ascorbic acid. The spectrophotometric determination of N-nitrososarcosine as nitrosyl bromide released into solution by the action of hydrogen bromide was hindered by the presence of powdered corn flakes.