The apparent totalN‐nitroso content of foods can be measured by a procedure based on chemical denitrosation and chemiluminescent detection of the eliminated nitric oxide. Procedures have been established which substantially reduce the ‘apparatus blank’ response to the denitrosating agent and allow total nitroso contents down to 10μg(N‐NO)/kg to be measured reproducibly on a 1‐g sample. Typically, duplicate analyses of samples containing 10–1000 μg (N‐NO)/kg differ by <15% of their mean. Potentially the method can be subject to some interference from compounds other thanN‐nitroso compounds, but at least in some commodities these interfering compounds do not exist in measurable amounts.