超高效液相色谱-串联质谱法测定罗非鱼中甲基睾酮残留  

Determination of methyltestosterone in Tilapia by UPLC-MS/MS

作　　者：张杨 张兵 李凯华 徐媛原 张微 肖曼 吴丹 张玲 ZHANG Yang;ZHANG Bing;LI Kaihua;XU Yuanyuan;ZHANG Wei;XIAO Man;WU Dan;ZHANG Ling(Shenzhen Institute of Quality&Safety Inspection and Research,Shenzhen 518055,China)

机构地区：[1]深圳市质量安全检验检测研究院,广东深圳518055

出　　处：《中国渔业质量与标准》2024年第1期27-34,共8页Chinese Fishery Quality and Standards

摘　　要：本研究建立了超高效液相色谱-串联质谱法测定罗非鱼(Oreochroms mossambcus)中甲基睾酮残留量的分析方法。罗非鱼样品匀浆,经含有1%甲酸的乙腈溶液提取,采用QuEChERS净化粉将提取液净化除杂,水浴氮吹浓缩,流动相溶解定容。样液经BEH C18色谱柱分离,以含0.1%甲酸的水溶液与甲醇流动相梯度洗脱,采用UPLC-MS/MS选择电喷雾ESI正离子多反应监测模式分析检测,内标法定量。结果表明:甲基睾酮在线性范围内线性关系良好,标准曲线相关系数为0.9995,方法检出限为0.30μg/kg,定量限为1.0μg/kg。3个添加水平(n=6)下罗非鱼基质的平均回收率为98.3%~103.0%,相对标准偏差为4.2%~8.8%。优化后方法灵敏度高,准确性好,前处理过程简单、快速,适用于开展罗非鱼中甲基睾酮残留的检测。In this study,a ultra performance liquid chromatography-tandem mass spectrometry method for the determination of methyltestosterone in tilapia was optimized and established.Tilapia samples were homogenized,extracted by acetonitrile solution containing 1.0%formic acid,purified by QuEChERS,concentrated by nitrogen blowing in water bath,and dissolved in mobile phase.The sample was separated on a BEH C 18 column and eluted with a gradient elution of aqueous solution containing 0.1%formic acid and methanol as mobile phase,using ESI positive ion multiple reaction monitoring mode in UPLC-MS/MS,and quantitative analysis was used with internal standard method.The results showed that methyltestosterone had a good linear relationship within the linear range.The correlation coefficient of the standard curve was 0.9995.The detection limit was 0.30μg/kg and the quantitative limit was 1.0μg/kg.At the different spiked levels(n=6)in tilapia substrate,the average recoveries were 98.3%to 103.0%and the relative standard deviation was 4.2%to 8.8%.The optimized method has high sensitivity,good accuracy,simple and rapid pre-treatment process,which is suitable for the detection of methyltestosterone residues in tilapia.

关 键 词：超高效液相色谱-串联质谱 罗非鱼 甲基睾酮 QUECHERS 激素残留 

分 类 号：S964[农业科学—水产养殖] O657.63[农业科学—水产科学]