A new methodology for extraction, pre-concentration and analysis of volatile nitrosamines in meat-derived products was developed and compared with conventional methods (Distillation and two-step solid-phase extraction). The samples (canned sausages, cured meat, luncheon and smoked meat) were treated with an aqueous sodium hydroxide (NaOH) by autoclaving at 121˚C for 10 min and extracted by liquid-liquid extraction with dichloromethane, then the nitrosamines were pre-concentrated 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 and gas chromatography with mass spectrometry detection was used as the confirmation technique. The newly invented autoclaving method allowed the determination of nitrosamine compounds at trace levels with limit of detection ranged from 0.077 to 0.18 ppb and quantitation limits were from 0.26 to 0.6 ppb for all nitrosamines, and found to be superior to the conventional ones, yielding approximately about 10%-20% increasing in the recovery compared with the mean recovery obtained when applying conventional methods.

The present work reports a rapid reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of seven volatile N-nitrosamines namely N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosodiproylamine (NDPA), N-nitrosodi butylamine (NDBA), N-nitrosopiperidine (NPIP) and N-nitrosopyrrolidine (NPYR) for monitoring food safety. A strategic experimental approach was implemented for the method development. The desired chromatographic separation was achieved on a Symmetry C18 (4.6 × 150 mm, 5 µm) column using gradient elution. The optimized mobile phase consisted of the 10 mM ammonium hydroxide pH = 8.9 and acetonitrile. The eluted compounds were monitored at 231 nm wavelength using spectrophotometric detector. The developed method separated seven compounds from each other within a run time of 10 min. The method is effective for the determination of presence of these carcinogenic compounds. The average extraction recovery of seven nitrosamines was found 84.5%; the precision of method was found less than 2.7% and accuracy was found between 95% -102.5%. The assay could be applied in food monitoring safety.

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˚C 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.