Scientific Publications by FDA Staff

J AOAC Int 2013 May-Jun;96(3):663-9

Development and Validation of a Method for the Simultaneous Determination and Confirmation of Melamine and Cyanuric Acid in Fish Kidney by LC/MS/MS.

Nochetto CB, Stine CB, Reimschuessel R

A method was validated to simultaneously determine and confirm melamine and cyanuric acid in fish kidneys by LC/MS/MS. This method is capable of detecting both compounds in a single procedure, whether present as free compounds or bound together as the melamine cyanurate complex in both channel catfish (Ictalurus punctatus) and rainbow trout (Oncorhynchus mykiss) kidneys. Residues are extracted with no additional cleanup and analyzed by LC/MS/MS using external standard calibration. The method is capable of quantifying residues over a range of 0.4 to 50 mu g/g. For both compounds and species of fish tested, the LOD is estimated to be 0.1 mu g/g and the LOQ 0.4 mu g/g. Recoveries and RSDs are 83 to 101% and 2 to 8%, respectively. In catfish, matrix effects are higher for melamine than cyanuric acid. In rainbow trout, similar matrix effects are found for both compounds.