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建立了鱼粉中孔雀石绿及其代谢物隐色孔雀石绿残留量的超高效液相色谱-串联质谱仪(UPLC-MS-MS)测定法。样品经乙腈提取,中性Al2O3固相小柱净化,超高效液相色谱C18柱分离,电喷雾正离子多反应模式(MRM)检测,内标法定量。方法的定量限为1.00μg/kg,线性范围为0.25～20.0μg/L。在1.00～20.0μg/kg的加标量下,孔雀石绿平均回收率范围为85.3%～104.4%,隐色孔雀石绿平均回收率范围为85.7%～101.4%,相对标准偏差均小于15%。方法适用于鱼粉样品中孔雀石绿残留的快速检测。
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method was developed for the determination of malachite green residues in malachite green and its metabolites. Samples were extracted with acetonitrile, neutral Al 2 O 3 solid phase cartridge, separated by ultra performance liquid chromatography C18 column, electrospray positive ion multiple reaction mode (MRM), and quantified by internal standard method. The limit of quantification was 1.00 μg / kg and the linear range was 0.25-20.0 μg / L. The average recoveries of malachite green in the range of 85.3% ~ 104.4% and the average recoveries of malachite green in the range of 85.7% ~ 101.4% and 1.00% ~ 20.0μg / kg were less than 15%. The method is suitable for the rapid detection of malachite green residue in fishmeal samples.