Hashimoto Juliana C, Paschoal Jonas A R, Queiroz Sonia C N, Ferracini Vera L, Assalin Márcia R, Reyes Felix G R
University of Campinas, Department of Food Science, School of Food Engineering, Campinas, SP, Brazil.
J AOAC Int. 2012 May-Jun;95(3):913-22. doi: 10.5740/jaoacint.11-140.
A simple method using LC/MS/MS was developed and validated to determine residues of malachite green (MG) and leucomalachite green (LMG) in fish fillet. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique was used to perform the sample preparation. The optimal extraction and cleanup conditions were established using an experimental design. The validation parameters obtained to determine both MG and LMG complied with the requirements established by regulatory agencies for the presence of such substances in fish, which establish that the method must attain, at least, a minimum required performance limit of 2 ng/g. The accuracy values ranged between 95 and 107%, and the precision values were lower than 11.2%. The method was used in the analysis of tilapia samples (n = 20) commercialized in Campinas, SP, Brazil. None of the samples presented detectable levels of MG or LMG residues.
开发并验证了一种使用液相色谱/串联质谱法(LC/MS/MS)测定鱼片中亚甲基蓝(MG)和无色亚甲基蓝(LMG)残留量的简单方法。采用改良的QuEChERS(快速、简便、廉价、有效、耐用和安全)技术进行样品制备。通过实验设计确定了最佳提取和净化条件。测定MG和LMG所获得的验证参数符合监管机构对鱼类中此类物质存在情况所规定的要求,该要求规定该方法必须至少达到2 ng/g的最低要求性能限值。准确度值在95%至107%之间,精密度值低于11.2%。该方法用于分析在巴西圣保罗州坎皮纳斯市商业化销售的罗非鱼样品(n = 20)。所有样品均未检测到MG或LMG残留量。