Simultaneous determination of melamine and cyanuric acid in foodstuffs by solid phase extraction-hydrophilic interaction chromatography-tandem mass spectrometry

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 - 2 500 mu g/L with the correlation coefficients r higher than 0. 99 and the limits of quantification were 25 mu g/kg and 50 mu g/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.