Abstract: A method based on solid phase extraction-liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of melamine and cyanuric acid in foodstuffs is presented. The melamine and cyanuric acid residues were extracted by acetonitrile and water, degreased by hexane, and the extract was cleaned-up by a mixed-mode solid phase-extraction column (MCT) of hydrophilic functional silica gel sorbent and cation exchange resin. The LC separation was performed on a hydrophilic interaction chromatograph, the melamine and cyanuric acid were determined by MS/MS in positive-negative switched electrospray ionization mode, multiple reaction monitoring (MRM) mode, and quantified by isotope internal standard method. The melamine and cyanuric acid were linear in the range of 10~2500 μg/L with the correlation coefficients (r) higher than 0.99, and the limits of quantification were 25 μg/kg and 50 μg/kg, respectively. The recoveries of melamine and cyanuric acid spiked in animal-derived foods, plant-derived foods, milk and milk products were in the range of 70.0%~129.6% and 70.0%~128.6%, respectively, with the relative standard deviations (RSD) of 1.4%~23.3% and 2.8%~18.7%, respectively. The method can meet the requirement for the determination of melamine and cyanuric acid in foodstuffs simultaneously.

Key words: cyanuric acid, foodstuffs, liquid chromatography-tandem mass spectrometry (LC-MS/MS) , melamine, solid phase extraction (SPE)