摘要
目的采用水相催化衍生化-液相色谱-紫外/荧光检测分析法,检测血中氟乙酸类杀鼠剂。方法血样经乙腈沉淀蛋白后,加入衍生化试剂4-溴甲基-7-甲氧基香豆素、催化剂四丁基溴化铵,在80℃水浴中衍生化反应120min,衍生产采用液相色谱-紫外/荧光检测分析。结果紫外检测法:氟乙酸根浓度在0.38～38.50μg/mL之间线性关系良好,最低检出限为0.10μg/mL;荧光检测法:氟乙酸根浓度在0.15～15.40μg/mL之间线性关系良好,最低检出限为0.050μg/mL。结论水相催化衍生化-液相色谱-紫外/荧光检测分析方法具有较好的灵敏度、准确性和精密度,可用于实际案例检测。
Objective To develop a method of analysis of monofluroacetate in human blood with precolumn derivatization in water by high performance liquid chromatography-ultraviolet detection/fluorescence detection. Methods The human blood samples were wiped off protein with acetonitrile, the supernatant was derivated in 80℃ water for 120min by using 4-Bromomethyl-7-methoxyeoumain as derivative reagent and tetrabutyl ammonium bromide as activator, the derivative was filtered through a 0. 45 μm membrane, and then were directly analyzed by high performance liquid chromatography-ultraviolet detection/fluorescence detection. Results The calibration curves showed good linearities in the rang of 0. 38 - 38.50μg/mL for ultraviolet detection and 0. 15 - 15. 401μg/mL for fluorescence detection, and the limits were 0. 10μg/mL and 0. 050μxg/ mL for ultraviolet detection and fuorescence detection, respectively. Conclusion The results show high accuracy, good precision and sensitivity, and it can be widely applied in the identification of monofluroacetate in cases.
出处
《中国法医学杂志》
CSCD
2012年第3期230-232,共3页
Chinese Journal of Forensic Medicine
基金
公安部应用创新项目(2011YYCXXJXY118)
辽宁省自然科学基金(201102246)
关键词
法医毒物分析
氟乙酸
液相色谱-荧光
血
杀鼠剂
forensic toxicological analysis
monofluroacetate
liquid chromatography-ultravioletdetection/fluorescence detection
blood
rodenticide
