As intermediates of atmospheric photochemical reactions, formaldehyde (HCHO) and glyoxal (CHOCHO) are often used as important tracers of atmospheric volatile organic compounds (VOCs), and monitoring and investigating their distribution and evolution plays an important role in regional air pollution monitoring. This study is based on the HCHO and CHOCHO data of the multi-axis differential optical absorption spectroscopy (MAX-DOAS) observation station in Qingyuan campus of Anhui University (117.18°E, 31.77°N), Hefei, China, from July to September in 2021. Firstly, the radiative transfer model SCIATRAN is selected as the forward model, and the vertical profiles of HCHO and CHOCHO are retrieved by the optimization estimation algorithm.Then, the distribution and evolution characteristics of HCHO and CHOCHO in this region are analyzed by comparing with the observation data of Tropospheric Monitoring Instrument (TROPOMI) carried on Sentinel-5 satellite and combining with the meteorological data. The strong correlation with TROPOMI observation data proves the high confidence level of the MAX-DOAS data. The results indicate that the HCHO profile near the ground has obvious diurnal variation, with higher levels at noon and at night. The weekly variation curve of HCHO is related to the activities of the residents, and it is shown that the HCHO concentration from Friday to Sunday is 20.13% higher than that of other working days, demonstrating an obvious weekend effect. Because CHOCHO and HCHO have different formation pathways as tracers, the ratio of CHOCHO to HCHO (RGF) is also studied to determine the emission source of VOC precursors. The analysis of RGF curve shows that biological VOC emissions are more prevalent in Hefei City. During the observation period, periods dominated by biological VOC emissions accounted for approximately 72.29% of the total observation time. This work explores the distribution and behavior evolution of HCHO and CHOCHO in Hefei, which provides a reference for the monitoring and prevention of air pollution in this area.