高效液相色谱-三重四级杆串联质谱法测定全血样中12种抗凝血类杀鼠剂

Determination of 12 kinds of anticoagulant rodenticides in whole blood by high performance liquid chromatography coupled with triple quadrupole mass spectrometry

目的建立高效液相色谱-三重四级杆串联质谱法检测鼠药中毒患者血液样品中12种抗凝血类杀鼠剂(杀鼠酮、杀鼠醚、氟鼠酮、杀鼠灵、溴敌隆、氯杀鼠灵、鼠得克、氯鼠酮、敌鼠、溴鼠灵、噻鼠酮、灭鼠优)的含量。方法样品经乙腈提取,上清液过0.22μm有机滤膜后上机。采用Waters BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm),以10 mmol乙酸铵-0.1%氨水和乙腈为流动相进行梯度洗脱,流速0.3 m L/min,柱温40℃,进样量5μL。多反应监测模式监测。结果 12种抗凝血类杀鼠剂加标回收率在80.5%~118.0%之间,批内相对标准偏差在1.4%~9.9%之间,检出限在0.1~0.3 ng/m L之间,定量限在0.3~1.0 ng/m L之间。结论该方法简单、灵敏、准确,能够快速检测中毒患者血液中抗凝血类杀鼠剂的含量。

Objective To establish a method for detection of 12 kinds of anticoagulant rodenticides（pindone, coumatetralyl, flocoumafen, warfarin, bromadiolone, coumachlor, difenacoum, chlorophacinone, diphacinone, brodifacoum, difethlalone and pyrinuron） in whole blood of rodenticides poisoning patients by high performance liquid chromatography coupled with triple quadrupole mass spectrometry. Methods The samples were extracted by acetonitrile, then the supernatant was filtered through 0.22 μm membrane microfilter for analysis. The sample was separated on an Waters BEH C_（18） column（2.1 mm×50 mm, 1.7 μm） with water contained 10 mmol/L ammonium acetate-0.1% ammonia and acetonitrile as mobile phase with gradient rlution, the flow rate was 0.3 m L/min, the temperature of column was 40 ℃ and the sample amount was 5 μL. The detection was carried out by multiple reaction monitoring. Results The recoveries of 12 kinds of anticoagulant rodenticides were 80.5%-118.0%, and the relative standard deviations（RSDs） were 1.4%-9.9%, the limit of detection were 0.1-0.3 ng/m L, and the limit of quantitation were 0.3-1.0 ng/m L. Conclusion This method is simple, sensitive and accurate. The results can be obtained quickly in whole blood of rodenticides poisoning patients.