As “fuel” for atmospheric photochemical reactions, volatile organic compounds (VOCs) play a key role in the secondary generation of ozone (O3) and fine particulate matter (PM2.5, an aerodynamic diameter ≤ 2.5 μm). To determine the characteristics of VOCs in a high-level ozone period, comprehensive monitoring of O3 and its precursors (VOCs and NOx) was continuously conducted in an industrial area in Shanghai from 18 August to 30 September 2021. During the observation period, the average concentration of VOCs was 47.33 ppb, and alkanes (19.64 ppb) accounted for the highest proportion of TVOCs, followed by oxygenated volatile organic compounds (OVOCs) (13.61 ppb), alkenes (6.92 ppb), aromatics (4.65 ppb), halogenated hydrocarbons (1.60 ppb), and alkynes (0.91 ppb). Alkenes were the predominant components that contributed to the ozone formation potential (OFP), while aromatics such as xylene, toluene, and ethylbenzene contributed the most to the secondary organic aerosol production potential (SOAFP). During the study period, O3, NOx, and VOCs showed significant diurnal variations. Industrial processes were the main source of VOCs, and the second largest source of VOCs was vehicle exhaust. While the largest contribution to OFP was from vehicle exhaust, the second largest contribution was from liquid petroleum gas (LPG). High potential source contribution function (PSCF) values were observed in western and southeastern areas near the sampling sites. The results of a health risk evaluation showed that the Hazard Index was less than 1 and there was no non-carcinogenic risk, but 1,3-butadiene, benzene, chloroform, 1,2-dibromoethane, and carbon tetrachloride pose a potential carcinogenic risk to the population.