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5 . 2018

Development and application of gas chromatography-mass spectrometry method for quantitive determination of volatile N-nitrosamines

Abstract

The article presents the results of experimental studies on the development of highly sensitive and selective chromatography-mass spectrometry technique for the determina­tion of 9 N-nitrosamines in food samples (sausage products) using distillation and an automatic solid-phase extraction system on Coconut cartridges for sample preparation. In the elaborated conditions of sample preparation (distillation and solid-phase extrac­tion) and chromatography-mass spectrometric analysis, we achieved a high recovery and efficiency of the separation of nine N-nitrosamines. The quantitation limit was at level of 0.0002 mg/kg with maximum error not exceeding 19%. The complex use of the distil­lation of N-nitrosamines with the addition of potassium hydroxide in combination with the optimal elution scheme for solid-phase extraction and concentrating the distillate into a Coconut carbon cartridge of 6 ml ensures the recovery of N-nitrosamines from the food product sample (sausage products) up to 93.2-100%. The process of approbation of the chromatography-mass spectrometric method in the samples of food products (sausage products) of various manufacturers revealed the content of N-nitrosamines in the con­centration range 0.00029±0.000055÷0.350±0.05 mg/kg. The conducted studies of the content of the sum of highly toxic N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) made it possible to disclose that in sample No. 5 the maximum allowable concentration was exceeded by 47 times, in samples No. 2 and 16, to 57.5 and 22.9 times and in sample No. 4 to 88 times, respectively.

Keywords:volatile N-nitrosamines, smoked meat products, gas chromatography-mass spectrometry method, solid-phase extraction

Voprosy pitaniia [Problems of Nutrition]. 2018; 87 (5): 102-110. doi: 10.24411/0042-8833-2018-10059. (in Russian)

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CHIEF EDITOR
CHIEF EDITOR
Viktor A. Tutelyan
Full Member of the Russian Academy of Sciences, Doctor of Medical Sciences, Professor, Scientific Director of the Federal Research Centre of Nutrition, Biotechnology and Food Safety (Moscow, Russia)

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