建立了膨化食品中三聚氰胺及其类似物的超高效液相色谱-四极杆-飞行时间质谱联用检测法.向样品中加入内标,用2.5%的甲酸提取,乙腈去除蛋白后直接上机分析.TOF采用V飞行模式,正离子模式下检测三聚氰胺、三聚氰酸-酰胺和三聚氰酸二酰胺,负离子模式下检测三聚氰酸.研究结果表明:4种化合物在HILIC色谱柱上分离良好,其中三聚氰胺、三聚氰酸在5~200ng-mL^-1质量浓度范围内线性良好;三聚氰酸二酰胺、三聚氰酸一酰胺在5-500ng·mL^-1质量浓度范围内呈良好的线性,方法绝对回收率达80.23%-96.52%,相对标准偏差小于6%,4种化合物的检测限均小于2ng·mL^-1.该方法无需复杂的前处理过程,适合于食品中三聚氰胺及其类似化合物超标样品的快速筛查和低含量定量分析.
An Ultra Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry (UPLC-Q-TOF-MS) method for residues of melamine and related compounds is adopted for use with puffed food. Four standard compounds as internal standard in puffed food are extracted with 2.5% aqueous formic acid. The cleaned-up extracts from the four compounds are identified as acetonitrile. The mass spectrometry is performed on reflective time-of-flight, and electrospray ionization is used in both the negative ion (cyanuric acid) and positive ion (melamine, ammeline and ammelide) modes. The results showing efficient separation of four compounds is achieved on ACQUITY UPLC HILIC column, indicating that the linear concentration range is within 0-200 ppb for melamine and cyanuric acid, and the linear concentration range of application is within 0-500ng-mL-1 for ammeline and ammelide. The absolute recovery ranges from 80.23% to 96.52%, and the relative standard deviation is found to be less than 6%, with low detection limit of 2 ng.mL-1. The UPLC-Q- TOF-MS method has been established for rapid screening and quantitative analysis of melamine and similar compounds in puffed food.