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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 for rapid analysis of aniline and benzidine in water by direct injection / ultra high pressure liquid chromatography with fluorescence detection was established. By studying the mobile phase, the pH value of water sample, the conductivity of water sample and the influence of filter material, the optimal experimental scheme was determined. The water samples were directly filtered through a 0.22 μm microporous membrane (PTFE) with acetonitrile-3.85 g / L ammonium acetate (25:75) as the mobile phase. The fluorescence detector (aniline λex / λem = 232 nm / 329 nm , Benzidine λex / λem = 292 nm / 383 nm) within 0.8 min. The linear correlation between aniline and benzidine in the range of 1.0 ~ 100.0μg / L was good with the correlation coefficients greater than 0.999 and the precision of the instrument (n = 10) were 0.4% and 0.5% respectively. The detection limit was S / N = 0.023 μg / L and 0.024 μg / L, respectively. The method was applied to determine the lower limit of quantification (S / N = 10) of 0.078 μg / L and 0.079 μg / L. The recovery was 86% -106%. The method has the advantages of simple pretreatment, low detection limit and fast analysis speed, and is suitable for the rapid detection of aniline and benzidine in water.