| HPLC-UVD/FLD法测定血中氟乙酸类杀鼠剂 |
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| 引用本文： | 陈学国,朱昱,姚伟宣,许英健.HPLC-UVD/FLD法测定血中氟乙酸类杀鼠剂[J].中国法医学杂志,2012,27(3):230-232. |
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| 作者姓名： | 陈学国 朱昱 姚伟宣 许英健 |
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| 作者单位： | 1. 中国刑警学院法医系,辽宁沈阳,110854
2. 中国刑警学院法医系,辽宁沈阳110854;浙江警察学院刑事科学技术系,浙江杭州310053 |
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| 基金项目： | 公安部应用创新项目(2011YYCXXJXY118);辽宁省自然科学基金(201102246) |
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| 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。
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| 关 键 词： | 法医毒物分析 氟乙酸 液相色谱-荧光 血 杀鼠剂 |
Determination of monofluoroacetate in human blood with precolumn derivatization by high performance liquid chromatography-ultraviolet detection/fluorescence detection |
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| Chen Xueguo
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Zhu Yu
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Yao Weixuan
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Xu Yingjian.Determination of monofluoroacetate in human blood with precolumn derivatization by high performance liquid chromatography-ultraviolet detection/fluorescence detection[J].Chinese Journal of Forensic Medicine,2012,27(3):230-232. |
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| Authors: | Chen Xueguo Zhu Yu Yao Weixuan Xu Yingjian |
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| Institution: | 1/1.China Criminal Police University,Shenyang 110854,China;2.Zhejiang Police University,Hangzhou 310053,China) |
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| Abstract: | 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-methoxycoumain as derivative reagent and tetrabutyl ammonium bromide as activator,the derivative was filtered through a 0.45μm 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 0.15~15.40μg/mL for fluorescence detection,and the limits were 0.10μg/mL and 0.050 μg/mL for ultraviolet detection and fluorescence 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. |
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| Keywords: | forensic toxicological analysis monofluroacetate liquid chromatography-ultraviolet detection/fluorescence detection blood rodenticide |
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