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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 establish a triple quadrupole LC / MS method for the simultaneous determination of 9 common anticoagulant rodenticides (warfarin, warfarin, natriuretic, chloropyridine, bromadiolone, Long, kill its battle, rat dextrose, chlorine warfarin). Methods The samples were extracted with acetonitrile and centrifuged at high speed and passed through a 0.2 μm membrane filter. The samples were directly separated by liquid chromatography. Nine kinds of rodenticides in the blood were detected by MRS in triple quadrupole mass spectrometer. Results The spiked recoveries of nine anticoagulant rodenticides in this method were 75.3% -109.8% with relative standard deviations of 2.6% -10.8%. At the concentrations of 0.05μg / L to 500.00μg / L The correlation coefficient> 0.998, the detection limit was 0.004μg / L ~ 1.200μg / L, the limit of quantification was 0.014μg / L ~ 4.000μg / L. Conclusion The method is simple, rapid, sensitive, qualitative confirmation and quantitative accurate. It can also confirm and quantify 9 rodenticides including broeturon, Dalong, chloropyril and warfarin in the blood at the same time, Requirements of rapid emergency detection of poisoning incidents.