Development and Validation of a Method for the Simultaneous Determination and Confirmation of Melamine and Cyanuric
Cristina B Nochetto1, Cynthia B Stine1, Renate ReimsChuessel1
1U.S. Food and Drug Administration, Center for Veterinary Medicine, Office of Research, 8401 Muirkirk Rd, Laurel, Maryland 20708.
Abstract:
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 microg/g. For both compounds and species of fish tested, the LOD is estimated to be 0.1 microg/g and the LOQ 0.4 microg/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.
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