[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.
Li
S
S
Institute of Chemical Defence, Testing and Analysis Center, Beijing, 102205.
Gu
H
H
Zheng
M
M
Zhan
Y
Y
D000627:Aminophenols / Q000737:chemistry*; D002384:Catalysis; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D004340:Drug Contamination / Q000517:prevention & control; D006865:Hydrogenation; D004364:Pharmaceutical Preparations / Q000032:analysis
D000627:Aminophenols; D004364:Pharmaceutical Preparations; C026729:4-aminophenol