QuEChERS/UPLC-MS/MS法测定水产品中孔雀石绿和结晶紫及其代谢物

摘要

A method for the determination of malachite green (MG),crystal violet (CV) and their metabolites residues leucomalachite green (LMG) and leucocrystal violet (LCV) in aquatic product was developed using QuEChERS combined with UPLC-MS-MS.The sample was extracted with acetonitrile and purified by EMR-Lipid.The target compounds were separated on an Agilent Eclipse Plus C18(1.8 μm,3.0 mm × 100 mm) column,and detected by tandem mass spectrometry with electrospray ionization in positive mode.The linear ranges were in the range of 0.2-10.0 μg/L and the correlation coefficients were all above 0.997.The average recoveries of 4 analytes in fish matrix at three spiked concentrations of 0.5,1.0,5.0 μg/kg ranged from 77.1％ to 106.6％,with relative standard deviations of 1.3％-4.3％.This method was simple and reliable,and could effectively remove the protein and fat in sample.Therefore,it is suitable for the determination of MG,CV and their leuco metabolites residues in aquatic product.%建立了水产品中孔雀石绿(MG)和结晶紫(CV)及其代谢物隐色孔雀石绿(LMG)和隐色结晶紫(LCV)残留的QuEChERS/UPLC-MS/MS分析方法.样品采用乙腈提取,改进的QuEChERS (EMR-Lipid)分散固相萃取净化,经Agilent Eclipse Plus C18(1.8 μm,3.0 mm×l00 mm)色谱柱分离,电喷雾串联四极杆质谱多反应监测正离子方式测定.4种分析物在0.2々 10.0 μg/L范围内线性关系良好,相关系数均大于0.997.鱼肉中4种分析物在0.5,1.0,5.0 μg/kg加标浓度水平下,回收率为77.1％ ～ 106.6％,相对标准偏差(RSD)为1.3％ ～4.3％.该方法简单、稳定、可靠,能有效去除样品中的蛋白质、脂肪等大分子杂质,可满足水产品中孔雀石绿、结晶紫以及隐色代谢物残留检测与确证的需要.