三重四级杆液质联用法快速测定全血样中9种抗凝血类灭鼠剂  

Quick determination of 9 anticoagulant rodenticides in whole blood by liquid chromatography-triple quadrupole tandem mass spectrometer

作　　者：贾玉珠[1] 蔡伟鹏[1] 陈丽惠[1] 白艳艳[1] 骆和东[1] 朱宝平[1] JIA Yu-zhu CAI Wei-peng CHEN Li-hui BAI Yan-yan LUO He-dong ZHU Bao-ping(Xiamen Municipal Center for Disease Control and Prevention, Xiamen, Fujian 361021, China)

机构地区：[1]厦门市疾病预防控制中心,福建厦门361021

出　　处：《中国卫生检验杂志》2016年第22期3196-3200,共5页Chinese Journal of Health Laboratory Technology

基　　金：厦门市科技计划社会发展项目资助(3502z20114038)

摘　　要：目的建立三重四级杆液质联用法,同时测定鼠药中毒患者血液样品中9种常见抗凝血类灭鼠剂(杀鼠醚、杀鼠灵、敌鼠钠盐、氯敌鼠、溴敌隆、大隆、杀它仗、鼠得克、氯杀鼠灵)。方法试样用乙腈提取,高速冷冻离心,过0.2μm滤膜,直接经液相色谱柱分离,在MRM模式下以三重四级杆质谱检测器测定血液中9种灭鼠剂。结果本方法中,9种抗凝血类灭鼠剂的空白血样加标回收率为75.3%~109.8%,相对标准偏差为2.6%~10.8%,在0.05μg/L^500.00μg/L的浓度内,相关系数>0.998,检出限为0.004μg/L^1.200μg/L,定量限为0.014μg/L^4.000μg/L。结论该法简单、快速、灵敏度高、定性确证和定量准确,可同时对血液中溴敌隆、大隆、氯敌鼠、杀鼠灵等9种灭鼠剂进行定性确证和定量测定,满足突发中毒事件快速应急检测的要求。Objective To develop a method for the simultaneous detection of 9 anticoagulant rodenticides（ Bromadiolone,Brodifacoum,Chlorophacinone,Warfarin,Bromadiolone,Brodifacoum,Flocoumafen,Neosorexa,Coumachlor） in the blood samples of rodenticides poisoning patients based on liquid chromatography- triple quadrupole tandem mass spectrometer（ LC / MS / MS）.Methods The samples were extracted by acetonitrile and centrifugated at high speed over 0. 2 μm filtration membrane,separated by liquid chromatography column,and then measured in MRM mode by LC / MS / MS method. Results The average recoveries of 9 anticoagulant rodenticides in blank blood samples were within 75. 3%- 109. 8%,and the relative standard deviations（ RSDs） were within 2. 6%- 10. 8%. The linearities of the method were within 0. 05 μg/L- 500. 00 μg/L,with the correlation coefficients（ r） greater than 0. 998. The limit of detection and quantification were within 0. 004 μg / L- 1. 200 μg / L and0. 014 μg / L- 4. 000 μg / L,respectively. Conclusion The method is simple,rapid,sensitive and specific. It＇s available to simultaneously detect 9 anticoagulant rodenticides with accurate qualitative and quantitative results,meeting the demand of rapid emergency detection of poisoning incidents.

关 键 词：三重四级杆液质联用法 中毒 全血 抗凝血类灭鼠剂 

分 类 号：O657.63[理学—分析化学]