A reference isotope dilution headspace GC/MS method for the determination of nitrite and nitrate in meat samples

A novel method for the determination of nitrite and nitrate in meat products is presented. The samples were ground and extracted in hot water with the presence of 15NO2- and 15NO3- internal standards. The solution was buffered with sodium bicarbonate and reacted with triethyloxonium tetrafluoroborate to convert nitrite and nitrate into EtNO2 and EtONO2. Such derivatives could be detected by headspace GC/MS in positive chemical ionisation mode with 0.05 mu g g(-1) NO2- and 1.0 mu g g(-1) NO3- LOD. The method was used for NO2- and NO3- quantitation in the 0.5-300 and 2.5-300 mu g g(-1) ranges. The method was applied for the analysis of fifteen meat products. Despite minimal sample preparation, the headspace sampling ensured a clean chromatography for over 135 analyses (throughput ten samples per hour). The proposed method offers selective GC/MS detection combined with high-precision isotope dilution calibration, it is suitable for metrological applications and can support regulations on meat safety (European Commission, 2011).