摘要
目的建立血中氟乙酸类杀鼠剂衍生化-液相色谱-电喷雾离子阱质谱分析方法。方法血样经乙腈沉淀蛋白后离心,上清液中加入衍生化试剂α-溴苯乙酮和催化剂四丁基溴化铵,在60℃水浴中加热90min,衍生化产物直接进行液相色谱-电喷雾离子阱质谱联用分析。结果血中氟乙酸根浓度在0.15μg/mL~15.40μg/mL之间具有良好的线性关系,最低检出限为0.020μg/mL。结论本文建立的方法操作简便、灵敏、快速,适用于刑事案件中氟乙酸类杀鼠剂的快速检验。
Objective To present a analysis method of monofluroacetate in human blood with pre-column derivatization and liquid chromatography and ion trap electro-spray mass spectrometry. Methods The human blood samples were wiped off protein with acetonitrile, the supernatant was devivated in 60 ℃water for 90 min using α-Br-acetophenone as derivative reagent and tetra- butyl ammonium bromide as activator, the derivative was filtered through a 0.45/,m membrane, and then was directly analyzed by liquid chromatography and ion trap electro-spray mass spectrometry. Results The calibration curve showed good linearities in rang of 0.15μg/mL-15.40μg/mL and the limit of detection was 0. 020μg/mL. Conclusion The Results showed this method is easy to operation and has good sensitivity, it can be widely applied in the identification of monofluroacetate for casework.
出处
《刑事技术》
2012年第1期21-23,共3页
Forensic Science and Technology
基金
公安部应用创新项目(No.2011YYCXXJXY118)
关键词
法医毒物分析
氟乙酸
液相色谱-质谱
血
杀鼠剂
forensic toxicology
monofluroacetate
liquid chromatography-mass spectrometry
blood
rodenticide