液相色谱-串联质谱法同时测定和确证鱼肾中三聚氰胺和氰尿酸的方法的建立与验证
Development and Validation of a Method for the Simultaneous Determination and Confirmation of Melamine and Cyanuric Acid in Fish Kidney by LC/MS/MS.
作者信息
Nochetto Cristina B, Stine Cynthia B, ReimsChuessel Renate
机构信息
U.S. Food and Drug Administration, Center for Veterinary Medicine, Office of Research, 8401 Muirkirk Rd, Laurel, Maryland 20708.
出版信息
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。
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