高效液相色谱-串联质谱法测定血液和尿液中12种杀鼠剂  

Determination of 12 rodenticides in blood and urine by HPLC-MS/MS

作　　者：游慧圆 刘云富[1] 谭广辉[1] 吴燕梅 YOU Huiyuan;LIUYunfu;TAN Guanghui;WU Yanmei(Huizhou Prevention and Treatment Center for Occupational Disease,Huizhou 516008,China;Huizhou Agricultural Product Quality and Safety Supervision and Testing Center,Huizhou 516008,China)

机构地区：[1]惠州市职业病防治院,广东惠州516008 [2]惠州市农产品质量安全监督检测中心,广东惠州516008

出　　处：《化学分析计量》2023年第9期17-22,共6页Chemical Analysis And Meterage

基　　金：广东省医学科学技术研究基金项目(B2022358)。

摘　　要：建立了血液和尿液样品中溴鼠灵、杀鼠醚、溴敌隆、杀鼠灵、氯杀鼠灵、克灭鼠、异杀鼠酮、氯敌鼠、敌鼠、鼠立死、安妥、毒鼠碱12种杀鼠剂同时快速测定的高效液相色谱-串联质谱。全血或尿液样品经涡旋振荡、乙腈萃取、高速离心后,上清液用氮吹浓缩后直接进样,经色谱柱分离,采用多反应监测(MRM)模式检测,以保留时间和特征离子及主要特征离子相对离子丰度定性,色谱峰外标法定量。12种灭鼠剂的质量浓度在一定质量浓度范围内与色谱峰面积的线性关系良好,相关系数为0.996~0.9997,方法检出限为4.4~14.8μg/L,样品加标回收率为81.2%~107.8%,相对标准偏差为0.7%~15.4%(n=6)。该方法适用于疑似鼠药中毒病人的全血和尿液样品中12种鼠药的同时定性、定量测定。A high performance liquid chromatography-tandem mass spectrometry method was established for the simultaneous and rapid determination of 12 rodenticides in blood and urine samples,including brodifacoum,coumatetralyl,bromadiolone,warfarin,coumachlor,coumafuryl,2-isovaleryl-1,3-indanedione,chlorophacinone,diphacinone,crimidine,1-naphthalenylthiourea and strychnine.The whole blood or urine samples were subjected to vortex oscillation,acetonitrile extraction,high speed centrifugation,followed by supernatant liquid nitrogen blowing and concentration followed by redissolution and direct injection.The samples were separated by chromatography column and detected by using multiple reaction monitoring(MRM)mode.The retention time and relative abundance of characteristic ions and main characteristic ions were used for qualitatively determination,while the external standard method by chromatograph peak area was used for quantitatively determination.The results showed that the mass concentration of 12 rodenticides had a good linear relationship with the chromatographic peak area within a certain concentration range,with the correlation coefficient between 0.996 and 0.9997.The detection limit of the method was between 4.4 and 14.8μg/L.The recovery rate of the sample was between 81.2%and 107.8%,and the relative standard deviation was between 0.7%and 15.4%.This method is suitable for the simultaneous qualitative and quantitative determination of 12 rodenticides in whole blood and urine samples of suspected rodenticide poisoning patients.

关 键 词：杀鼠剂 高效液相色谱-串联质谱法 血液 尿液 

分 类 号：O657.63[理学—分析化学]