High performance liquid chromatography analysis of p-aminophenol synthesized by nitrobenzene transfer hydrogenation using formic acid as hydrogen sourceEI北大核心CSCD

Qualitative analysis of the main by-product of 4-hydroxybenzamide in the synthesis of p-aminophenol bynitrobenzene transfer hydrogenation with formic acid as hydrogen source was carried out by electrospray ionization mass spectrometry. The reaction system was quantitatively analyzed by high performance liquid chromatography. The chromatographic conditions were shown as followsShim pack VP-ODS column250 mm× 4.6 mm5 μµmdetection wavelength of 254 nmVmethanolVbuffer solution=114.8 mmol/L sodium dihydrogen phosphate solution1.9 mmol/L dibasic sodium phosphate solutionas the mobile phase and the flow rate of 0.8 mL/min with a column temperature of 35. Nitrobenzenep-aminophenolaniline and formylaniline in the reaction system were quantitatively analyzed by standard curve method with methyl N-phenylcarbamate as internal standard. The correlation coefficientsR2were 0.99930.99950.9998 and 0.9992 for these analytes respectively. The relative standard deviations RSDs were less than 1.0% 0.3% 0.2% and 0.4% respectively. The recoveries were in the ranges of 95.5%-102.6%101.2%-104.8%95.1%-99.8% and 95.7%-101.1%respectively. This method can be used for the simultaneous determination of main and by-products in the transfer hydrogenation of nitrobenzene with formic acid as hydrogen source. © 2022, Youke Publishing Co.,Ltd. All rights reserved.