Miniaturized and improved method for Apparent Total N-Nitroso Compounds determination in beer

Tomáš Vrzal; Michaela Malečková; Jana Olšovská

doi:10.18832/kp2021.67.498

Authors

Tomáš Vrzal Research Institute of Brewing and Malting, Lípová 511/15, 120 00 Prague 2, Czech Republic
Michaela Malečková Research Institute of Brewing and Malting, Lípová 511/15, 120 00, Prague 2, Czech Republic
Jana Olšovská Research Institute of Brewing and Malting, Lípová 511/15, 120 00, Prague 2, Czech Republic

DOI:

https://doi.org/10.18832/kp2021.67.498

Keywords:

nitrosamines, nitroso compounds, ATNC, chemiluminescence detection, miniaturization

Abstract

A miniaturized and improved method for Apparent Total Nitroso Compounds determination in liquid matrices was developed. The main improvement is based on a miniaturized and modified apparatus for chemical denitrosation of nitroso compounds by hydrogen bromide in a glacial acetic acid mixture. The reaction is carried out in a teflon reaction coil while the reaction product, gaseous nitric oxide, is drifted to a chemiluminescence detector by the flow of argon together with a vacuum obtained by the detector's oil pump. The apparatus significantly increased the efficiency of the Apparent Total N-Nitroso Compounds determination (compared to the previous method), specifically, the dead volume of the apparatus was significantly decreased, and the effect of the reverse reaction was eliminated as well. The apparatus shortens the analysis time (1.4 min/injection), further it provides a lower detection limit (3 μg(N-NO)/l), quantification limit (10 μg(N-NO)/l), and method uncertainty (15%), and is simpler for the operation.

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