急性杀鼠剂中毒检材的液相色谱串联质谱法快速确证  

Quick confirmation of rodenticides in poisoning samples by liquid chromatography tandem mass spectrometry

作　　者：张英[1] 蔡志斌[1] 徐小燕[1] 赖建辉[1] 刘金明[1] 刘红河[2] 

机构地区：[1]深圳市龙岗区疾病预防控制中心,广东深圳518172 [2]深圳市疾病预防控制中心,广东深圳518055

出　　处：《中国卫生检验杂志》2017年第17期2456-2460,共5页Chinese Journal of Health Laboratory Technology

基　　金：深圳市卫生计生系统科研项目(20133222)

摘　　要：目的针对不同样品类别优化前处理方法和仪器方法,建立食糜和生物体液等基质复杂中毒检材中14种杀鼠剂(毒鼠强、氟乙酰胺、氟乙酸、溴敌隆、溴鼠灵、杀鼠灵、杀鼠迷、杀鼠酮、灭鼠优、氯敌鼠、鼠得克、氟鼠灵、敌鼠、噻鼠酮)的液相色谱串联质谱(LC-MS/MS)快速确证方法。方法样品中氟乙酸经丙酮水萃取,其余13种杀鼠剂经乙酸乙酯或乙腈萃取,氮吹浓缩后用初始流动相复溶,直接上LC-MS/MS,以杀鼠灵-D5为内标,在不同色谱及质谱条件下进行定性确证与定量检测。结果 14种杀鼠剂的定量下限为0.1μg/L^50μg/L,对方便面、果汁、全血、尿液4类样品进行加标回收试验,回收率为71.9%~103.5%,相对标准偏差(RSD)为3.76%~10.30%。结论该方法简单、快速、准确、灵敏,在实际中毒样品检测中,能达到定性及定量的要求,适用于毒鼠强、氟乙酸、溴敌隆等14种急性杀鼠剂中毒检测的快速质谱确证。Objective To optimize the pretreatment procedures and the instrument conditions against diverse matrices and analytes and to establish a quick confirmation method for the detection of 14 rodenticides（ tetramine,fluoroacetamide,fluoroacetic acid,bromadiolone,brodifacoum,warfarin,coumatetralyl,pindone,pyrinuron,chlorophacinone,difenacoum,flocoumafen,diphacinone and difethialone） in both chyme and biological matrices by liquid chromatography with tandem mass spectrometry（ LC-MS/MS）. Methods Fluoroacetic acid was extracted by acetone-water and the rest 13 rodenticides were extracted by either ethyl acetate or acetonitrile. The extracted solutions were then concentrated by nitrogen sweeping and the residues were redissolved in the mobile phase solution. Qualitative confirmation and quantitative detection were completed by LC-MS/MS with warfarin-D5 as internal standard. Qualitative identification and quantitative detection were carried out under different chromatographic and mass spectrometric conditions. Results The lower limit of quantitation for 14 rodenticides were within 0. 1 μg/L-50 μg/L. Standard addition experiments were carried out for the analytes in instant noodles,juice,whole blood and urine,respectively. The recoveries for 14 rodenticides in the above matrices ranged from 71. 9% to 103. 5% with the relative standard deviations（ RSDs） within 3. 76%-10. 30%. Conclusion The established analytical procedure is simple,rapid,accurate and sensitive. It can be employed for qualitative and quantitative assay of practical poising samples,and it is more suitable for quick MS confirmation for 14 rodenticides such as tetramine,fluoroacetic acid and bromadiolone.

关 键 词：杀鼠剂 急性中毒 液相色谱串联质谱 确证 

分 类 号：O657.63[理学—分析化学]