LC-MS/MS法同时测定水产品中孔雀石绿、结晶紫及其代谢物残留量

Research on Simultaneous Determination of Malachite Green and Gentian Violet and their Metabolites Residues in Aquatic Products by LC-MS/MS

[目的]建立测定水产品中孔雀石绿(MG)、结晶紫(GV)及其代谢产物残留量的液相色谱-串联离子阱质谱仪测定法(LC-MS/MS)。[方法]将样品中残留的MG或GV用硼氢化钾还原为其相应的代谢产物隐色孔雀石绿(LMG)或隐色结晶紫(LGV),经净化预处理,用串联离子阱质谱在电喷雾-全扫描二级质谱(MS/MS)模式进行质谱测定,与HPLC方法测定结果比对验证。[结果]在55件可疑样品中,用本法测定有46件为阳性,9件为假阳性,本法测定结果满意。[结论]采用LC-MS/MS法测定水产品中MG、GV及其代谢产物含量,结果准确,灵敏度高。

[Objective] To establish the determination method of malachite green（MG）and gentian violet（GV） and their metabolites residues in aquatic products by LC-MS/MS.[Methods] Of MG and GV residues in samples with potassium borohydride reduction of their respective metabolites as leuco-MG（LMG） and leuco-GV（LGV）.Samples were pretreated and then detected by using a liquid chromatography coupled electrospray ionization（ESI ＋） and Ion trap mass spectrometry-full scan MS/MS mode.The method was well validated and good results,comparing with HPLC method.[Results] Of 55 suspected samples detected by HPLC,46 were positive,9 were false positive,and the method can get good results.[Conclusion] The determination of MG and GV and their metabolites content in aquatic products by LC-MS/MS,the results are accurate,reliable and high sensitivity.