超高效液相色谱-串联质谱快速测定水产品中孔雀石绿、结晶紫及其代谢物残留量

建立了超高效液相色谱-串联质谱（UPLC-MS/MS）测定水产品中孔雀石绿（MG）、结晶紫（CV）及其代谢物隐色孔雀石绿（LMG）和隐色结晶紫（LCV）残留量的快速、准确检测方法。该法在SN/T1768-2006快速检测方法的基础上,采用空白样品添加不同质量浓度标准溶液的方式绘制校准曲线,并以氘代孔雀石绿（D5-MG）和氘代隐色孔雀石绿（D6-LMG）为内标进行检测,从而大大提高了定量的准确性。结果表明,MG、CV、LMG和LCV4种待测物在0～10.0ng·mL^-1范围内线性关系良好（R〉0.99）,方法检出限均为0.1μg·kg^-1。在加标量为0.5和1.0μg.kg-1水平下4种待测物平均回收率在92.1%～111.0%之间,测定结果的相对标准偏差为2.2%～9.5%。此外,该法在FAPAS国际能力验证中得以证实,改进后的方法快速且准确,能满足水产品出口检测要求。

Rapid residue determination of malachite green, crystal violet and their metabolites in aquatic products by UPLC-MS/MS

We developed a rapid and accurate method by UPLC-MS/MS to determine the residue of malachite green （MG）,crystal violet （CV） and their metabolites （LMG and LCV） in aquatic products.Based on the rapid method of SN/T 1768-2006,standard curves were made by adding standard solutions of different concentrations to the blank samples,and D5-MG and D6-LMG were used as internal standards,which improved the accuracy of determination.The results show that MG,CV,LMG and LCV have a good linear correlation within the range of 0～10.0 ng·mL^-1 （R〉0.99）,and the detection limits of the method are all 0.1 μg·kg^-1.The average recoveries at fortification of 0.5 and 1.0 μg·kg^-1 range from 92.1%to 111.0% with relative standard deviations （RSD）varying from 2.2% to 9.5%.Furthermore,the rapid and accurate improved method is also proved by FAPAS Proficiency Test to meet the export testing requirements of aquatic products.