衍生化-液相色谱-质谱联用测定血中氟乙酸类杀鼠剂

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。

Determination of monofluoroacetate in human blood by pre-column derivatization and liquid chromatographymass spectrometry

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 tetrabutyl ammonium bromide as activator,the derivative was filtered through a 0.45μm 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.