摘要
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.
作者
殷跃
晋朋姣
李彦威
YIN Yue;JIN Peng- jiao;LI Yan-wei(Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024, Chin)
出处
《化学试剂》
CAS
北大核心
2018年第7期653-657,共5页
Chemical Reagents
基金
山西省自然科学基金资助项目(201601D102016)
关键词
高效液相色谱法
同时测定
硝基苯
苯胺
对氨基苯酚
high performance liquid chromatography
simultaneous determination
nitrobenzene
aniline
p-aminophenol