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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 pre-treatment methods and apparatus for different sample types, 14 kinds of rodenticides (tetramisotram, fluoroacetamide, fluoroacetic acid, bromadiolone, bromodexapril (LC-MS / MS) was developed for the rapid and rapid identification of human immunodeficiency virus Confirmation method. Methods Fluoroacetic acid was extracted by acetone water and the remaining 13 rodenticides were extracted with ethyl acetate or acetonitrile. After the concentration of nitrogen was concentrated, the sample was reconstituted with the original mobile phase and directly on LC-MS / MS. The concentration of warfarin-D5 Internal standard, under different chromatographic conditions and mass spectrometry qualitative confirmation and quantitative detection. Results The lower limit of quantitation of 14 rodenticides was 0.1μg / L ~ 50μg / L. The spiked recoveries of instant noodles, fruit juice, whole blood and urine were 71.9% ~ 103.5%. The relative standard deviations (RSD) was 3.76% ~ 10.30%. Conclusion The method is simple, rapid, accurate and sensitive. It can meet the qualitative and quantitative requirements in the detection of actual poisoning samples and is suitable for the rapid mass spectrometry detection of 14 acute rodenticides poisoned by tetramine, fluoroacetic acid and bromadiolone Confirmed.