高效液相色谱法测定水中硝基苯和苯胺含量

Determination of Aniline and Nitrobenzene in Water by High Performance Liquid Chromatography

建立了高效液相色谱直接进样快速分析水样中苯胺和硝基苯的方法。操作条件为:进样量5μL;流速1 mL/min;流动相为V(乙腈)∶V(3.85 g/L乙酸铵+3 g/L乙酸)=65∶35混合液;苯胺用荧光分析,λex/λem=280/340 nm;硝基苯用紫外分析,波长为262 nm;分离柱为Eclipse XDB2-C8柱(150 mm×4.6 mm,5μm);测试时间为3.2 min;样品前处理方法:1.0 mL水样与1.0 mL甲醇混匀,用微孔滤膜(0.45μm,有机系)过滤。苯胺和硝基苯标准曲线的线性相关系数均>0.999。测试苯胺、硝基苯时,仪器精密度分别为1.56%和0.13%。方法的回收率在89%～110%之间。仪器对苯胺和硝基苯的检出上限分别是50和200 mg/L;苯胺和硝基苯的方法检出限分别是18和21μg/L。

A method was developed to measure aniline and nitrobenzene in water sample by high performance liquid chromatography. The optimum condition was as follows： injection volume was 5 μL, flow rate was 1 mL/min, mobile phase was V（acetonitrile） ： V（3.85 g/L ammonium acetate ＋ 3.0 g/L acetic acid） = 65：35, aniline was determined by fluorescence, λex/λ em = 280/340 nm, nitrobenzene was determined by ultraviolet absorption at 262 nm, separation column was Eclipse XDB2-C8（150 mm × 4.6 mm, 5 μm）, test time was 3.2 min. Before the measurement, a mixture of 1 mL water sample and 1 mL methanol, was filtered through mierofiltration membrane. Linear correlation coefficients of aniline and nitrobenzene standard curves were 〉0. 999. The relative standard deviation of eight parallel injections was 〈 2%. Recovery rate of the method was in the range of 89% -110%. The instrumental detection limit of aniline and nitrobenzene was 50 and 200 mg/L, respectively. The method detection limit of aniline and nitrobenzene was 18 and 21 μg/L, respectively.