A method has been devised for the determination of nitrite at low level that is directly applicable to food or other dried matrices without prior extraction. Nitric oxide released from nitrite through the action of acetic acid is determined using a chemiluminescence analyser. The limit of detection is approximately 0.02 microgram, the coefficients of variation being 5.7 and 8.2% using 0.1 and 0.05 microgram of sodium nitrite, respectively. The chemiluminescence analyser response is diminished when water in excess of 0.5 ml is present in the assay system unless hydrogen bromide in acetic acid is used instead of acetic acid alone. The application of the method to the direct determination of nitrite in freeze-dried cod fish has indicated a content of 0.25 mg NaNO2 per kg, equivalent to 0.050 mg per kg of the original undried material.