摘要
为了快速实现同时测定鱼体中3类禁限用镇静剂,本文建立了鱼体中3种卡因类、1种非巴比妥类和6种苯二氮卓类镇静剂的高效液相色谱-串联质谱多残留同时测定方法。样品先经乙腈提取、低温高速离心处理,再经高效液相色谱快速分离,由联用的三重四极杆/复合线性离子阱质谱仪检测,能同时测定鱼体中10种镇静剂残留量。方法的线性范围为0.2~20.0μg/L,相关系数均>0.9990,对鱼肉的定量限为1.0μg/kg;以空白鲤鱼肌肉为样品,在1.0、2.0和5.0μg/kg这3个质量分数水平下测定了10种镇静剂的平均回收率,结果为86.5%~118.5%,相对标准偏差为2.2%~7.7%。表明本文所建的方法简便、快速、灵敏和准确,适用于水产品中10种镇静剂残留量的常规检测。
In order to quickly determine three types of prohibited and restricted sedatives in fish,a rapid high performance liquid chromatography-tandem mass spectrometry method was explored for the simultaneous determination of three types of cocaine,one type of non-barbiturates,and six types of benzodiazepine tranquilizers in fish samples.The sample was extracted with acetonitrile,rapidly purified by low-temperature high-speed centrifugation,fast separated by ultra-performance liquid chromatography,and detected by online-coupled triple quadrupole/composite linear ion trap mass spectrometer.The linear working curves were measured in the concentration range of 0.2 to 20.0μg/L,with linear correlation coefficients all higher than 0.9990,and quantification limits at 1.0μg/kg in fish.The recovery was measured by spiking 10 tranquilizer standards into carp muscle tissue at three levelsof 1.0,2.0 and 5.0 μg/kg,giving averaged data all within the range between 86.5% and 118.5%,withrelative standard deviations between 2.2% and 7.7%. The method is validated to be simple,rapid,efficient,sensitive and accurate,being usable as a routine method for the determination of 10 types oftranquilizers in aquatic products.
作者
李芹
文宇鹏
霍文迪
刘欢
穆迎春
李晋成
LI Qin;WEN Yupeng;HUO Wendi;LIU Huan;MU Yingchun;LI Jincheng(Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture,Chinese Academy of Fishery Sciences,Beijing 100141;College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306)
出处
《首都师范大学学报(自然科学版)》
2025年第6期1-8,共8页
Journal of Capital Normal University:Natural Science Edition
基金
中央级公益性科研院所基本科研业务费(2024D001)
中国水产科学研究院科技创新项目(2020TD75)
现代农业产业技术体系建设专项基金项目(CARS-48)。
关键词
水产品
镇静剂
高效液相色谱-串联质谱法
aquatic products
tranquilizer determination
high performance liquid chromatographytandem mass spectrometry
