Determination of volatile nitrosamines in meat products by microwave-assisted extraction and dispersive liquid-liquid microextraction coupled to gas chromatography-mass spectrometry.

In this study, an efficient, sensitive, and rapid method based on microwave-assisted extraction coupled with dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography–mass spectrometry for determination and quantification of seven nitrosamines (NAs) in heated meat products (sausage and salami) was developed. At extraction stage, nitrosamines were extracted from sausage and salami samples with 10 mL of a hydrolyzing solvent using microwave at 500 MHz for 1.5 min. Effective parameters on DLLME, such as volumes of extraction and disperser solvents, pH, and salt addition, were optimized using response surface methodology based on central composite design. This technique provided acceptable repeatability in the range of 3.5–5.4 % for spiked samples. The recoveries of NAs were in the range 83.9–109.4 %. Limits of detection and limits of quantification for NAs in the real samples were within the ranges of 0.11–0.48 and 0.41–1.45 ng g−1, respectively. Good linear ranges were obtained for seven NAs in the range of 0.1–200 ng mL−1, with the coefficient (R
 2) higher than 0.99. The merit figures, compared with other methods, showed that new proposed method is an accurate, precise, and reliable sample pretreatment method that substantially reduces sample matrix interference and gives very good enrichment factors (126–152).

Rapid determination of nitrosamines in sausage and salami using microwave-assisted extraction and dispersive liquid–liquid microextraction followed by gas chromatography–mass spectrometry

Introduction N-nitrosamines are formed in food as a result of natural chemical interactions, but mainly through food processing activity. Most are potent carcinogens and their determination is therefore of considerable importance. They exist in various chemical forms and have been measured by colorimetric and spectroscopic methods following gas or liquid chromatography or as a total N-nitroso group by measurement of chemically released nitric oxide.

Objectives To provide an overview of the available methods for the analysis of N-nitrosamines in food that includes recently developments.

Methods The literature was reviewed from the discovery of the N-nitrosamine problem and the introduction on the N-nitroso-specific detector.

Results The evaluation shows that analytical detection methods for volatile N-nitrosamines in food have changed little since the introduction on the N-nitroso-specific detector and that research into the occurrence and formation of both non-volatile N-nitrosamines and the apparent total N-nitroso content (ATNC) have declined. Methods for measuring the apparent total N-nitroso content have not been improved significantly in recent years.

Conclusion Modern sample extraction techniques and mass spectrometric methods for the volatile N-nitrosamines have been applied more extensively to water analysis and offer a good opportunity to improve the determination of these carcinogens in food and make the analysis more widely available. Developments in liquid chromatography-mass spectrometry should provide an avenue for renewed interest in non-volatile N-nitrosamines, and could help with the identification of novel compounds whose presence is suggested by the high apparent total N-nitroso content of some foods.

The determination of N‐nitrosamines in food

Determination of some carcinogenic contaminants in food

In this study, various fast food samples, including raw meat, cured meat,
grilled meat, fried meat, smoked meat and canned meat products, were analyzed for the determination of the seven volatile
N-nitrosamines. The samples were treated with an aqueous sodium hydroxide
(NaOH) by autoclaving at 121&degC for 10 min and extracted by liquid-liquid
extraction with dichloromethane, and then the nitrosamines were pre-concentrated by using activated silica. Then, gas
chromatography coupled with flame ionization detector was used for the
separation and determination of the different nitrosamines contained in a real
sample. The applied method allowed the determination of nitrosamine compounds
at trace levels with limit of detection ranging from 0.077 to
0.18 ppb, and quantitation limits were from
0.26 to 0.60 ppb for all nitrosamines. The total concentrations of the seven nitrosamines
in the studied meat samples ranged from 2.60 to 13.28 μg/kg.

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Determination of Seven Volatile N-Nitrosamines in Fast Food

Nine laboratories participated in a collaborative study of a method for determining 6 nitrosamines, dimethylnitrosamine, diethylnitrosamine, dibutylnitrosamine, nitrosopiperidine, nitrosopyrrolidine, and nitrosomorpholine, in the 5-17 ppb range. The coefficients of variation for repeatability were 10.8, 8.5, 10.4, 8.5, 8.7, and 7.8% with corresponding coefficients of variation for reproducibility of 16.4, 12.0, 13.6, 10.8, 11.2, and 10.3% and recoveries of 89.6, 91.6, 84.7, 90.0, 89.6, and 88.1%, respectively. The method was adopted official first action.

M Robach

Papers

Mineral oil vacuum distillation method for nitrosamines in fried bacon, with thermal energy analyzer: collaborative study.