超高压液相色谱荧光检测法快速测定水中痕量苯胺与联苯胺

Determination of Trace Aniline and Benzidine in Environmental Water by Ultrahigh-pressure Liquid Chromatography with Fluorescence Detection

建立了直接进样/超高压液相色谱荧光检测法快速分析水中苯胺和联苯胺的新方法。通过研究流动相、水样pH值、水样电导率和滤器材质的影响,确定了最优化的实验方案。水样直接通过0.22μm微孔滤膜(聚四氟乙烯材质)过滤,以乙腈-3.85 g/L醋酸铵(25∶75)为流动相,荧光检测器(苯胺λex/λem=232nm/329 nm,联苯胺λex/λem=292 nm/383 nm)在0.8 min内完成分析。苯胺和联苯胺在1.0～100.0μg/L范围内线性关系良好,相关系数均大于0.999,仪器精密度(n=10)分别为0.4%和0.5%,方法检出限(S/N=3)分别为0.023μg/L和0.024μg/L,方法定量下限(S/N=10)为0.078μg/L和0.079μg/L,方法回收率为86%～106%。该方法具有前处理简单、方法检出限低、分析速度快等优点,适用于水体中苯胺和联苯胺的快速检测。

A new method was developed for the determination of aniline and benzidine in environmental water by direct injection and ultrahigh-pressure liquid chromatography（UPLC） with fluorescence detection.Through the investigation of mobile phase,pH value and conductivity of water samples,and filter materials,the optimum conditions were obtained.Under the optimal conditions,water samples were filtered through the microfiltration membrane（0.22 μm,PTFE）,and analyzed by UPLC using acetonitrile-3.85 g/L ammonium acetate（25 ∶ 75） as mobile phase in 0.8 min.The fluorescence detection wavelengths were set at λex/λem=232 nm/329 nm for aniline and λex/λem=292 nm/383 nm for benzidine.Good linear relationships were obtained in the range of 1.0-100.0 μg/L for aniline and benzidine with correlation coefficients more than 0.999.The relative standard deviations（n=10） of 10.0 μg/L aniline and benzidine were 0.4% and 0.5%,respectively.Recoveries for the method were in the range of 86%-106%.The detection limits（S/N=3） for aniline and benzidine were 0.023 μg/L and 0.024 μg/L,and the quantitation limits（S/N=10） were 0.078 μg/L and 0.079 μg/L,respectively.The method was simple,sensitive and rapid,and could be applied in the detection of aniline and benzidine in environmental water.