电还原邻硝基苯酚合成邻氨基苯酚的高效液相色谱分析法

High Performance Liquid Chromatography for the Synthesis of o-Aminophenol by Electroreduction o-Nitrophenol

建立了一种反相高效液相色谱法同时测定邻硝基苯酚和邻氨基苯酚的新方法。采用Shim-pack VP-ODS(250 mm×4.6 mm,4.6μm)色谱柱,选用纯甲醇为流动相,以285 nm为检测波长,流速为0.8 m L/min,柱温为35℃,以外标法进行定量分析。实验结果表明,邻硝基苯酚和邻氨基苯酚的质量浓度在1.0~40.0μg/m L范围内呈良好的线性关系,其相关系数分别为r=0.999 5(n=9)和r=0.999 8(n=9),测定其在10.0、20.0和30.0μg/m L这3个不同质量浓度下的方法精密度,其相对标准偏差分别≤1.28%和≤1.04%。将本方法应用于以邻硝基苯酚为原料电解合成邻氨基苯酚反应液的分析,其加标回收率分别在93.0%~105.6%和90.6%~106.2%之间,相对标准偏差分别≤3.75%和≤1.44%。实验结果表明,该方法可用于邻硝基苯酚和邻氨基苯酚两种组分的同时测定。

A new method for the simultaneous determination of o-nitrophenol and o-aminophenol by reversed-phase high performance liquid chromatography was developed. HPLC was carried out on a VP-ODS Shim-pack column（250 mm × 4. 6 mm,4. 6μm）,using pure methanol as mobile phase and the detection was performed by UV detector at 285 nm,of which flow rate was 0. 8m L/min and the column temperature was 35 ℃ through the external standard method. The results showed that the o-nitrophenol and o-aminophenol concentration ranged from 1. 0 μg/m L to 40. 0 μg/m L can obtained a good linear relationship,the correlation coefficient were 0. 999 5（n = 9） and 0. 999 8（n = 9） respectively.Determination of the 10. 0 μg/m L,20. 0 μg/m L,30. 0 μg/m L three different concentration sample solutions of precision,the relative standard deviations were no more than 1. 28% and 1. 04%,respectively.It has been used to determine the product in the process of electrolytic synthesis of o-aminophenol with o-nitrophenol as raw material,the recoveries were between 93. 0% ~ 105. 6% and 90. 6% ~ 106. 2%,the relative standard deviations were no more than 3. 75% and 1. 44%.The results show that the method can be used for simultaneous determination of o-nitrophenol and o-aminophenol.