This study aims to evaluate the concentration of biomarkers for heavy metals and volatile organic compounds (VOCs) for the residents living in the Gwangyang industrial complex to compare with residents in the residential area as a control. A total of 810 healthy adults participated in this study, and their urinary and blood samples were analyzed for metals, including As, Pb, Cd, or Hg, and VOC compounds. All study participants also completed questionnaire surveys to collect more detailed information on personal lifestyles, dietary and drinking habits, residential housings types, and their health conditions. The geometric means of urinary levels of Cd were 1.06 g/g creatinine for those living in the vicinity of Gwangyang industrial complex and 1.41 g/g creatinine for those in residential areas (p<0.05). Furthermore, urinary mean levels of Hg were 1.39 μg/g creatinine in the industrial area and 1.23 μg/g creatinine in the control area, respectively. The concentrations of individual VOCs in blood were significantly different between the two population groups. Therefore, urinary levels of Cd and Hg were significantly higher in the local residents compared to the Gwangyang industrial areas. A further study is needed to identify adverse health effects due to environmental exposures to heavy metals, VOCs, and other pollutants in the Gwangyang industrial complex areas in the future.