A new methodology for extraction, pre-concentration and analysis of nitrosamines in meat derived products was developed. The samples (canned sausages) were distilled in vacuum steam and the nitrosamines were pre-concentrated by solid-phase extraction with active carbon. Then, micellar electrokinetic chromatography 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 method allowed the determination of nitrosamine compounds at trace levels with relative standard deviation ranging from 4.0 to 22%.