Rapid Solid-Phase Extraction Method for the Detection of Volatile Nitrosamines in Food

Abstract

A rapid solid phase extraction (SPE) method was developed to analyze volatile N-nitrosamines (NAm) in foods. The currently used vacuum distillation technique is time and solvent consuming and is cumbersome for multiple analyses. Our objective was to develop a robust analytical method to measure the eight most common volatile NAm found in foods. The extraction procedure was based on two consecutive extraction/concentration steps using Extrelut and Florisil SPE. The amounts of food sample and solvent required were reduced compared to the conventional vacuum distillation method without affecting the sensitivity which was at a 0.3 ppb detection limit. A greater confidence in the analyte detection was obtained by the use of a capillary GC column, instead of the conventionally used open packed column, prior to thermal energy analyzer (TEA) detection. Another advantage of our method is the use of commercial cartridges, which ensures reproducibility and standardization of the method for multiple analyses. An application of the SPE method to a survey of volatile NAm content in sausages and dried milk powder revealed no contamination (<0.3 ppb) of either of these food samples.

Effect of plant polyphenols and ascorbic acid on lipid oxidation, residual nitrite and N‐nitrosamines formation in dry‐cured sausage

“…The other N-nitrosamines (NMEA, NDPA, NDBA, NPIP, NMOR and NDPheA) were not found or were under the level of detection. The contents of N-nitrosamines found here were similar to those reported recently with other meat products (Raoul et al, 1997;Drabik-Markiewicz et al, 2009;Campillo et al, 2011). The content of NDEA was very low and was not detected at the end of ripening.…”

“…In the current study, the total N-nitrosamine contents ranged from 5.72 to 7.98 lg kg À1 and were less than 10 lg kg À1 in the sausages at the end of ripening. The contents of N-nitrosamines found here were similar to those reported recently with other meat products (Raoul et al, 1997;Drabik-Markiewicz et al, 2009;Campillo et al, 2011). The residual nitrite content (mg NaNO 2 kg À1 sample) during ripening of dry-cured sausages containing ascorbic acid, green tea polyphenol (GTP) or grape seed polyphenol (GSP).…”

Comportamento eletroquímico da N-nitrosotiazolidina ácido carboxílico sobre eletrodos de ouro e mercúrio

“…6 Todavia, os métodos cromatográficos têm sido os mais utilizados na determinação de nitrosaminas em matrizes diversas, onde a cromatografia líquida de alta eficiência e a cromatografia gasosa tem sido empregadas para a determinação das nitrosaminas não voláteis e voláteis, respectivamente. Os detectores mais utilizados em ambas as técnicas têm sido o de quimiluminescência (TEA -Thermal Energy Analyzer), uma vez que esse é seletivo para compostos que contêm o grupo N-nitroso [7][8][9] e o de massas. 10,11 Entretanto, as técnicas cromatográficas associadas ao detector de quimiluminescência ou ao espectrômetro de massa requerem alto investimento inicial e, em função disto, poucas indústrias no Brasil controlam seus produtos quanto à presença de nitrosaminas.…”

Determination ofN-nitrosamines in processed meats by liquid extraction combined with gas chromatography-methanol chemical ionisation/mass spectrometry

“…Furthermore, the K-D concentration step is challenging because VNAs are highly volatile. The extraction of NAs in foods by simple methods that can reduce the procedure time and generate the least amount of organic solvents is definitely needed but poses challenges, as shown by some studies (Raoul et al 1997;Andrade et al 2005). Determination of NAs from pork sausages using solid-phase micro-extraction (SPME) was carried out by Andrade et al (2005).…”