Method for group determination of total N-nitroso compounds and nitrite in fresh gastric juice by chemical denitrosation and thermal energy analysis

Abstract

A method for the determination of total N-nitroso compounds (NOC) and nitrite in fresh human gastric juice is described, which is based on earlier methods. A freshly obtained gastric juice sample is injected directly into refluxing ethyl acetate containing glacial acetic acid, HCl and HBr to determine the total concentration (A) of nitrite, total NOC and thermo- and acid-labile thermal energy analyser (TEA)-responsive compounds (TAC). Another fresh sample of the same juice (with or without the addition of sulfamic acid) is injected directly into refluxing ethyl acetate containing glacial acetic acid and HCl for determining the TAC level (B) and the total level (C) of nitrite and TAC. The NO released from nitrite, TAC and NOC is detected by TEA acting as a chemiluminescence detector. The differences between A and C and between C and B represent the concentrations of total NOC and nitrite, respectively. The method is rapid, reproducible (relative standard deviation 1–6%) and sensitive (detection limit 1.0 pmol). The behaviour of nitrite and NOC in the analytical system was studied and relevant techniques for the direct analysis of fresh gastric juice samples and for stabilization of fresh samples have been developed.