超高效液相色谱法直接快速测定环境水样中硝基苯和苯胺

建立了超高效液相色谱直接快速测定环境水样中硝基苯和苯胺的分析方法。取900μL水样与100μL乙腈混匀,用微孔滤膜(0.2μm,有机系)过滤。采用1.7μm小颗粒填料的BEH phenyl柱,以乙腈/醋酸铵溶液为流动相,硝基苯和苯胺分别用紫外和荧光检测器检测,分析时间仅1.1 min。硝基苯和苯胺的线性范围分别是0.485～4850μg/L和0.495～1978μg/L,方法检出限分别是0.194μg/L和0.099μg/L,相关系数均在0.995以上。硝基苯9.70μg/L、194μg/L、1940μg/L三个浓度水平回收率在98.3%～101%,相对标准偏差在1.11%～2.03%。苯胺9.89μg/L、198μg/L、1978μg/L三个浓度水平回收率在98.6%～104%,相对标准偏差在0.75%～5.85%。与传统液相分析方法相比,本方法线性范围更宽,灵敏度更高;直接进样简化了前处理环节,减少采样体积和有机试剂的使用;分析效率高,适用于地下水、地表水等多种水质样品中痕量到常量范围的硝基苯和苯胺快速测定。

Direct and Rapid Determination of Nitrobenzene and Aniline in Environmental Water by Ultra Performance Liquid Chromatography

A rapid and direct analytic method has been established for the determination of nitrobenzene and aniline in environmental water samples by Ultra Performance Liquid Chromatography(UPLC).The mixture of 900 μL water and 100 μL acetonitrile was filtered through a microfiltration membrane(0.2 μm,organic).The UPLC analysis program has been improved by using a BEH phenyl separation column,filled with 1.7 μm BEH particles,and the mobile phase used acetonitrile ammonium acetate.Nitrobenzene and aniline were detected respectively at the ultraviolet(262 nm) wavelength and fluorescence(λex/λem=280 nm/340 nm) respectively.The whole analysis program took only 1.1 min.The linear range of nitrobenzene and aniline were 0.485-4850 μg/L and 0.495-1978 μg/L,respectively.The detection limits of the methods were 0.194 μg/L and 0.099 μg/L,respectively,and the correlation coefficients were both above 0.995.The recoveries of nitrobenzene in three concentration levels of 9.70 μg/L,194 μg/L and 1940 μg/L were 98.3%-101%,and the relative standard deviation was in the range of 1.11%-2.03%.The recoveries of aniline in three concentration levels of 9.89 μg/L,198 μg/L and 1978 μg/L were 98.6%-104%,and the relative standard deviation was in the range of 0.75%-5.85%.Compared with the traditional liquid chromatography analysis methods,this method is suitable for the determination of nitrobenzene and aniline in groundwater,surface water and other water samples,with the advantages of being simple,rapid,sensitive,highly efficient,with a wide linear range and less sample and reagent consumption.