A simple extraction followed by LC separation on a HILIC column and MS/MS detection in negative and positive Electrospray Ionization using an API 3200™ LC/MS/MS System enables the quantitation of Melamine and Cyanuric Acid below 1μg/kg. The method provides an extra degree of confirmation through the use of Multiple Reaction Monitoring(MRM) ratios.Future investigation will include the optimization of recovery by adjusting pH during sample preparation and the use of isotopically labeled internal standards to correct for possible matrix effects during ionization.