摘要
目的建立血液中4类(7种)鼠药(毒鼠强、氟乙酸根、溴敌隆、大隆、杀鼠灵、杀鼠醚、氟鼠灵)的超高效液相色谱-高分辨质谱(UPLC-HRMS)快速检测方法。方法采用乙腈为蛋白沉淀剂,用PLD+净化柱或有机微孔过滤膜净化提取液,用UPLC-HRMS对血液中的4类(7种)鼠药进行定性定量检测。分析采用Luna Omega PS C18(2.1mm×100mm,3μm)色谱柱,质谱扫描方式为负离子的全扫描/实时二级质谱扫描(Full MS/ddMS^(2))模式,一级全扫描(m/z 50~750)分辨率为70000,二级扫描(ddMS^(2))分辨率为17500。结果毒鼠强、氟乙酸根、溴敌隆、大隆、杀鼠灵、杀鼠醚、氟鼠灵的检出限均为50ng/mL,3个添加水平下的回收率为85.3%~94.7%,日内相对标准偏差(RSD)为3.4%~11%(n=6),日间相对标准偏差(RSD)为5.6%~13%(n=6)。结论使用本方法可同时准确测定血液中的4类(7种)鼠药。
Objective To develop an analytical method for simultaneous determination of seven rodenticides(TETS,fluoroacetic acid,bromadiolone,brodifacoum,warfarin,coumatetralyl and flocoumafen)(categorized into 4 major kinds)in whole blood through ultra-high performance liquid chromatography-high resolution mass spectrometry(UPLC-HRMS).Methods The samples were treated with acetonitrile to precipitate protein,successively extracted through purification of PLD+polymer column or organic microporous filter membrane.Luna Omega PS C18 chromatographic column(2.1mm×100mm,3μm)was adopted for chromatographic separation with gradient elution.The analytes were detected under the mode of negative-ion ESI in full MS/ddMS^(2).Results Detection limits(LODs)of the seven rodenticides varied among 10~50 ng/mL.The recoveries ranged from 85.3%~94.7%at three spiked levels in whole blood.The intra-day relative standard deviation(RSD)was 3.4%~11%(n=6),with the inter-day’s being 5.6%~13%(n=6).Conclusion This method is both qualitative and quantitative,capable of simultaneous and accurate screening of seven rodenticides in whole blood.
作者
徐琛
李晓飞
张云峰
应剑波
XU Chen;LI Xiaofei;ZHANG Yunfeng;YING Jianbo(Hangzhou Institute of Criminal Science and Technology,Hangzhou 310000,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)
出处
《刑事技术》
2021年第4期365-369,共5页
Forensic Science and Technology
基金
杭州市农业与社会发展科研主动设计项目(20190101A08)。
