体液中氟乙酰胺SPE-GC/MS检测

目的　利用GC/MS与固相萃取 (SPE)技术相结合 ,开发血和尿样中氟乙酰胺鼠药的GC/MS定量分析新方法 ,并用于实际案例检测。方法　选择乙酰胺为内标 ,通过比较不同固相柱的萃取效率和不同条件对回收率的影响 ,优化用于血和尿样中氟乙酰胺萃取的固相柱和提取条件 ,利用氟乙酰胺与乙酰胺质谱图的分子离子峰面积之比与氟乙酰胺浓度的定量关系 ,建立血和尿样中氟乙酰胺鼠药的GC/MS定量分析新方法。结果　用硅胶柱萃取 ,峰面积之比与氟乙酰胺浓度在 5 0～ 90 μg/ml范围呈线性关系 ,检测限为 1 0 μg/ml。血样中氟乙酰胺检测的平均回收率达 91 6% ,标准偏差小于 7 3 %。结论　此法对实际样品的测定证明可满足氟乙酰胺鼠药中毒的定性定量要求。

Determination of fluoroacetamide in body fluid using solid-phase extraction-gas chromatography/mass spectrometry technique

Objective To develop a new quantitative analytical method for determination of fluoroacetamide,a kind of raticides,in blood and urine samples using solid-phase extraction combined with GC/MS.Methods Using acetamide as the internal standard,extraction column and extraction conditions of fluoroacetamide from blood and urine samples were optimized by comparing the extraction efficiency of different solid-phase extraction columns and the effects of experimental conditions on recovery.By means of the quantitative relation between the ratio of characteristic ion peak areas of fluoroacetamide to acetamide a novel analytical method for determination of fluoroacetamide concentration was established by quantitative GC/GM technique.Results The ratio was proportional to the concentration of fluoroacetamide ranging from 5.0 to 90μg/ml with silica gel column extraction,and the detection limit was estimated to be 1.0μg/ml.The average recovery of fluoroacetamide in blood sample was 91.6%.The standard deviation was less than 7.3%.Conclusion The analytical results were in conformity with those obtained by the classical method,which could satisfy the requirement for quantitative measurement of fluoroacetamide in samples from practical cases.