超高效液相色谱-串联质谱法检测鱼类中孔雀石绿、结晶紫及其代谢物  

Detection of malachite green,crystal violet and its metabolites in fish by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：师真[1] 李文廷[1] 张瑞雨[1] 欧利华[1] 梁孟军[1] 赵丽[1] SHI Zhen;LI Wen-Ting;ZHANG Rui-Yu;OU Li-Hua;LIANG Meng-Jun;ZHAO Li(Kunming Center for Disease Control and Prevention,Kunming 650228,China)

机构地区：[1]昆明市疾病预防控制中心,昆明650228

出　　处：《食品安全质量检测学报》2020年第9期2861-2865,共5页Journal of Food Safety and Quality

摘　　要：目的建立超高效液相色谱-串联质谱法测定鱼类中孔雀石绿、结晶紫及其代谢物的分析方法。方法本方法依据GB/T 19857-2005,样品用乙腈提取,分散固相萃取净化管净化后,采用色谱柱分离。样品经过离子化后进入质谱仪中,以水和乙腈为流动相,电喷雾正离子化模式(electrospray ionization,ESI+)和多反应检测(multiple reaction monitoring,MRM)扫描模式进行测定,同位素内标法定量。结果孔雀石绿和结晶紫及其代谢产物在0.2~2.0 ng/mL浓度范围内,线性关系良好(r>0.999),检出限均为0.5μg/kg。在0.5~2.0μg/kg水平内,目标物质的平均加标回收率在99.71%~112.86%之间,相对标准偏差均不超过13%。对72份鱼类样品进行检测,隐性孔雀石绿的检出率为1.38%,其余均未检出。结论该方法定量准确、分析时间短,适用于鱼肉中孔雀石绿和结晶紫及其代谢物残留量的定量检测。Objective To establish a method for the determination of malachite green,crystal violet and its metabolites in fish by ultra performance liquid chromatography-tandem mass spectrometry.Methods Based on GB/T 19857-2005,the samples were extracted with acetonitrile and purified by d-SPE purification tube.The samples were separated by chromatographic column,and then entered into the mass spectrometer after ionized.Water and acetonitrile were used as the mobile phase,electrospray ionization(ESI+)and multiple reaction monitoring(MRM)scanning mode were used to determine the samples,and the internal standard method was used for quantitative analysis.Results Malachite green,crystal violet and their metabolites showed a good linear relationship(r>0.999)in the concentration range of 0.2-2.0 ng/mL,with detection limits of 0.5μg/kg.Within the range of 0.5-2.0μg/kg,the average recoveries of target substances were between 99.71%and 112.86%,and the relative standard deviations were not more than 13%.72 fish samples were detected,the detection rate of leucomalachite green was 1.38%,the others were not detected.Conclusion The method is accurate and time-consuming.It is suitable for the quantitative determination of malachite green,crystal violet and their metabolites residues in fish.

关 键 词：超高效液相色谱-串联质谱法 孔雀石绿 隐性孔雀石绿 结晶紫 隐性结晶紫 鱼类 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]