超高效液相色谱-串联质谱法同时检测水产品中孔雀石绿、结晶紫及其代谢物的残留

Simultaneous determination of malachite green,crystal violet and their metabolites residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

目的建立同时检测水产品中孔雀石绿（malachite green,MG）、隐色孔雀石绿（leucomalachite green,LMG）、结晶紫（crystal violet,CV）和隐色结晶紫（leucocrystal violet,LCV）等残留量的超高效液相色谱-串联质谱（UPLC-MS/MS）的分析方法。方法样品经乙腈提取,经中性氧化铝柱净化,采用超高效液相色谱-串联质谱法以电喷雾正离子化模式（electrospray ionization,ESI＋）和多反应监测（multiple reaction monitoring,MRM）扫描模式进行测定,以同位素内标法定量。同时考察了基质效应对检测结果的影响。结果水产品中MG、LMG、CV和LCV的基质效应不同,其中LCV的基质效应最为明显,加标回收率较低（约50%）。MG、LMG、CV和LCV 4种物质在0.2~5.0 ng/mL浓度范围内呈良好线性,相关系数均大于0.999,方法检出限为0.1~0.2μg/kg。MG、LMG和CV的加标回收率为93.5%~109.2%,相对标准偏差为5.4%~9.6%（n=6）。结论该方法仪器分析时间短、定量准确、检出限低,可用于检测水产品中MG、LMG、CV和LCV的残留量。

Objective To establish a method for simultaneous determination of malachite green（MG）,leucomalachite green（LMG）,crystal violet（CV） and leucocrystal violet（LCV） residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.Methods The samples were extracted with acetonitrile,cleaned up with neutral alumina column,and then detected by UPLC-MS/MS with electrospray ionization（ESI＋） mode and multiple reaction monitoring（MRM） mode.Isotope internal standards were used for quantification.Meanwhile the matrix effects were also observed.Results Different matrix effects existed in 4 kinds of analytes,especially in the LCV.The recovery of LCV was low（about 50%）.MG,LMG,CV,and LCV had good linear relationships in the range of 0.2~5.0 ng/mL（r0.999）.The limits of detection（LOD） were 0.1~0.2μg/kg.The recoveries of MG,LMG and CV were ranged from 93.5%to 109.2%.The relative standard deviations（RSDs） were 5.4%~9.6%（n=6）.Conclusion The method is rapid,accurate and sensitive,which is suitable for the detection of MG,LMG,CV and LCV residues in aquatic products.