高效液相色谱-串联质谱法同时测定草鱼中6种阳离子染料残留量

Simultaneous Determination of Six Cationic Dyes by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了同时测定草鱼中孔雀石绿、隐色孔雀石绿、结晶紫、隐色结晶紫、亚甲基蓝和新亚甲基蓝6种阳离子染料残留量的高效液相色谱-串联质谱（HPLC-MS/MS）方法。样品经乙腈和缓冲溶液提取,用二氯甲烷萃取及中性氧化铝固相萃取柱净化。选择反应监测（SRM）正离子模式检测,内标法定量。孔雀石绿、隐色孔雀石绿、结晶紫、隐色结晶紫、新亚甲基蓝和亚甲基蓝的定量限均为0.2μg/kg。添加0.2-10μg/kg水平时加标回收率达到75.0%-98.5%,相对标准偏差为3.2%-9.1%。

A method for simultaneous determination of malachite green,leucomalachite green,crystal violet,leucine crystal violet,methylene blue and new methylene blue residues in grass carp by high performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted with a mixture of acetonitrile and buffer,cleaned up with dichloromethane and a neutral alumina solid phase extraction cartridge,and detected by a selective reaction monitoring（SRM）mode using positive ions of HPLC-MS/MS and internal standard quantification.The detection limits（LOD）of the method were 0.2μg/kg for malachite green,leucomalachite green,crystal violet,leucocrystal violet,methylene blue and new methylene blue,respectively.The recovery rates were 75.0%-98.5%,and the relative standard derivations（RSD）ranged from 3.2%to 9.1%.