反相高效液相色谱法测定对氨基酚及其相关化合物

 用反相高效液相色谱法测定对氨基酚及其杂质４，４′－二氨基二苯醚和苯胺的含量。选择了最佳色谱条件，提供了各组分的紫外光谱图。对氨基酚、苯胺和４，４′－二氨基二苯醚的线性范围分别为５～２５０，５～１５０和０．２～１２０ｍｇ／Ｌ，检测限分别为０．１，０．６和０．６ｎｇ。所建立的方法已应用于超声催化氢化法合成反应的跟踪监测和工业样品的分析鉴定，结果令人满意。

Studies on Determination of p Aminophenol and Its Related Compounds Prepared with Catalytic Hydrogenation by Reversed Phase High Performance Liquid Chromatography

Catalytic hydrogenation of nitrobenzene with supported palladium catalyst is a new method to produce p-aminophenol. p-Aminophenol, aniline and 4,4'-diaminodiphenyl ether obtained from this method were determined by reversed phase high performance liquid chromatography. The factors, e.g., concentration of methanol, pH and ionic strength which could affect separation efficiency were studied. UV spectra of p-aminophenol, aniline and 4,4'-diaminodiphenyl ether were recorded. Good separation was performed by using a 100 mm x 4.6 mm column with 5 microm Hypersil ODS, a mixture of 60% aqueous 8.0 mmol/L KH2PO4 buffered to 6.5 with 4.0 mmol/L Na2HPO4 and 40% methanol as mobile phase at a flow rate of 1.0 mL/min, and UV spectrophotometric detector at 232 nm wavelength. The calibration curves of p-aminophenol, aniline and 4,4'-diaminodiphenyl ether have good linearity over concentration range of 5-250, 5-150 and 0.2-120 mg/L, respectively. Minimum detectable limits at a signal-to-noise ratio of 2 were 0.1, 0.6 and 0.6 ng. This method has been applied to analysis of the reaction products of ultrasonic catalytic hydrogenation and industrial samples with good results and reproducibility.