利用高效液相色谱-串联质谱法同时测定养殖鱼中孔雀石绿、结晶紫及其代谢物残留量

Simultaneous Determination of Malachite Green,Crystal Violet and Their Metabolite Residues in Cultured Fish by High Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:建立一种利用高效液相色谱-串联质谱仪的方法,测定养殖鱼中孔雀石绿(Malachite Green,MG)、结晶紫(Crystal Violet,CV)、隐色孔雀石绿(Leuco Malachite Green,LMG)及隐色结晶紫(Leuco Crystal Violet,LCV)残留量,为了解辖区市售水产品中禁用兽药残留情况,为食品安全风险评估提供可靠依据。方法:本方法依据《2017年国家食品污染和有害因素风险监测工作手册》监测方法,样本经乙腈提取,中性氧化铝固相萃取小柱净化,液相色谱分离后进入质谱仪,以电喷雾正离子化模式(ESI+)和多反应检测(Multi Reaction Detection,MRM)扫描模式测定,同位素内标法定量。结果:养殖鱼中孔雀石绿(MG)、结晶紫(CV)及其代谢物共4种成分在0.25~10.00 ng/mL线性关系良好,相关系数r均大于0.998,检出限均为0.5μg/kg,在0.5~2.0μg/kg加标回收率在83.8%~109.7%。对40份养殖鱼(大菱鲆、乌鳢和鳜鱼)进行检测,其中2份隐色孔雀石绿(LMG)有检出,检出率为5%,其他成分无检出。结论:该方法简单快速、定量准确、灵敏度高,可用于养殖鱼中孔雀石绿、结晶紫及其代谢物残留定量测定。

Objective:To establish a method for the simultaneous determination of malachite green(MG),crystal violet(CV),leuco malachite green(LMG)and leuco crystal violet(LCV)residues in cultured fish using high performance liquid chromatography-tandem mass spectrometer method.To understand the banned veterinary drug residues in aquatic products sold in the jurisdiction and provide a reliable basis for food safety risk assessment.Method:According to“2017 National Food Pollution and Harmful Factor Risk Monitoring Work Manual”,samples were extracted with acetonitrile,purified by neutral alumina solid phase extraction cartridge,separated by liquid chromatography,and then entered into the mass spectrometer,determined by electrospray positive ionization mode(ESI+)and multireaction detection(MRM)scanning mode,and isotope internal standard method Quantitative.Conclusion:The four components of malachite green(MG),crystal violet(CV)and their metabolites in cultured fish have a good linear relationship within the concentration range of 0.25~10.00 ng/mL,the correlation coefficient r is greater than 0.998,and the detection limit is 0.5μg/kg,the recovery rate of standard addition within 0.5~2.0μg/kg is between 83.8%~109.7%.Forty cultured fish(turbiny turbot,black snakehead and mandarin fish)were tested,of which 2 leuco malachite green(LMG)were detected,with a detection rate of 5%,and no other ingredients were detected.Conclusion:The method is simple,fast,accurate and sensitive,and can be used for the quantitative determination of malachite green,crystal violet and their metabolite residues in cultured fish.