Nochetto Cristina B, Stine Cynthia B, ReimsChuessel Renate
U.S. Food and Drug Administration, Center for Veterinary Medicine, Office of Research, 8401 Muirkirk Rd, Laurel, Maryland 20708.
J AOAC Int. 2013 May;96(3):663-669. doi: 10.5740/jaoacint.12-303.
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 and rainbow trout 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 μg/g. For both compounds and species of fish tested, the LOD is estimated to be 0.1 μg/g and the LOQ 0.4 μg/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.
建立了一种通过液相色谱-串联质谱法（LC/MS/MS）同时测定和确证鱼肾脏中三聚氰胺和氰尿酸的方法。该方法能够在单一程序中检测这两种化合物，无论是以游离化合物形式存在，还是在斑点叉尾鮰和虹鳟鱼的肾脏中以三聚氰胺-氰尿酸复合物形式结合存在。无需额外净化即可提取残留物，并使用外标校准通过LC/MS/MS进行分析。该方法能够在0.4至50μg/g的范围内对残留物进行定量。对于所测试的两种化合物和鱼类品种而言，估计检出限（LOD）为0.1μg/g，定量限（LOQ）为0.4μg/g。回收率和相对标准偏差（RSD）分别为83%至101%和2%至8%。在鲶鱼中，三聚氰胺的基质效应高于氰尿酸。在虹鳟鱼中，则发现两种化合物的基质效应相似。
