电还原硝基苯合成对氨基苯酚的高效液相色谱分析法

High Performance Liquid Chromatography of Electro-reduction of Nitrobenzene to p-Aminophenol

建立了一种对电还原硝基苯反应产物进行检测的高效液相色谱法。选用Shim-pack VP-ODS色谱柱（250 mm×4.6mm,4.6μm）,流动相为60%甲醇溶液,检测波长为235 nm,流速为1.0 m L/min,柱温为25℃,采用标准曲线法对硝基苯、苯胺和对氨基苯酚进行定量分析。得到了对氨基苯酚、硝基苯和苯胺的标准曲线,三者在5.0~55.0μg/m L浓度范围内,其相关系数分别为r=0.999 5（n=11）、r=0.999 4（n=11）和r=0.999 5（n=11）,且此方法的精密度良好,其相对标准偏差分别≤1.7%、≤2.2%和≤2.4%。利用此方法检测电还原硝基苯反应的产物,其加标回收率分别为92.0%~103.4%、90.8%~107.3%和93.8%~108.2%,表明此方法可用于硝基苯、苯胺和对氨基苯酚3组分的同时测定。

A high performance liquid chromatography（ HPLC） method was developed for the detection of the electro-reduced nitrobenzene reaction product.The experiment was performed on a Shim-pack VP-ODS column（ 250 mm×4. 6 mm,4. 6 μm） with a mobile phase of 60% methanol at a detection wavelength of 235 nm and a flow rate of 1. 0 mL/min with a column temperature of 25 ℃.Nitrobenzene,aniline and p-aminophenol were quantitatively analyzed by standard curve method.The calibration curves of p-aminophenol,nitrobenzene and aniline were obtained from the experiment. In the range of 5. 0 ～ 55. 0 μg/mL,the correlation coefficients were r = 0. 999 5（ n = 11）,r = 0. 999 4（ n = 11） and r = 0. 999 5（ n = 11）,and the precision of this method was good with the relative standard deviations of ≤1. 7%,≤2. 2% and ≤2. 4%,respectively.Using this method to detect the product of electro-reduction of nitrobenzene,the spiked recoveries were 92. 0% ～ 103. 4%,90. 8% ～ 107. 3% and 93. 8% ～ 108. 2%,respectively,indicating that this method can be used for simultaneous determination of nitrobenzene,aniline and p-aminophenol 3 components.