论文部分内容阅读
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 determine fluoroacetic acid rodenticides in blood by catalytic aqueous derivatization-liquid chromatography-ultraviolet / fluorescence detection and analysis. Methods The blood sample was precipitated by acetonitrile, then the derivatization reagent 4-bromomethyl-7-methoxycoumarin and the catalyst tetrabutylammonium bromide were added into the blood sample for derivatization reaction at 80 ℃ for 120 min. The liquid phase Chromatography - UV / fluorescence detection analysis. Results UV detection: The calibration curve was linear between 0.38 and 38.50 μg / mL with the detection limit of 0.10 μg / mL. The fluorescence detection method was linear with the concentration of fluoroacetate between 0.15 and 15.40 μg / mL Good relationship, the minimum detection limit of 0.050μg / mL. Conclusion The aqueous phase catalytic derivatization - liquid chromatography - UV / fluorescence detection and analysis method has good sensitivity, accuracy and precision, which can be used in the actual case detection.