The paper evaluates the presence of methyl xanthine compounds: caffeine, theophylline, theobromine used as ingredients in carbonated soft drinks or as color and flavor ingredients in alcoholic beverages. The active components extracted from the selected products (coffee, tea, drinks) was separated and identified chromatographically using plates with silica nano -Sil NH2 / UV-254, mobile phase ethanol - water (50: 1, 50: 3, 50: 5; 50: 7; v / v) and 60 F254 plates, mobile phase acetone-toluene-chloroform (40:30:30 v / v). Separated caffeine and identified by TLC was analyzed using a HelWet Packard 5890 Gas Chromatograph equipped with MS 5972 mass detector and spectral library to confirm identification. This simple and rapid TLC, GC / MS instrumental method is useful in controlling traces of methyl xanthine compounds in food as a food safety measure.is useful in controlling traces compound of food products containing methylxanthines as a food safety measure.