Oxygenated volatile organic compounds (OVOCs) are pervasive indoor air pollutants that negatively impact human health. Formaldehyde (HCHO), acetaldehyde (ACET), glyoxal (GLY), and methylglyoxal (MGLY) are among the OVOCs most frequently detected in indoor environments at concentrations associated with adverse respiratory effects, such as asthma. Only recently has it become possible to detect and quantify these recalcitrant compounds at trace concentrations using solid-phase microextraction (SPME) with on-fiber derivatization. Strategies for reducing human exposure to these harmful compounds are not yet well understood. Adsorption of HCHO, ACET, GLY, and MGLY to activated carbon is one potential treatment strategy evaluated in this study using SPME with on-fiber derivatization. The sensitivity and linear range of three detection methods-GC-FID, -MS, and -electron capture detection (ECD)-are compared. Additionally, adsorption capacities of HCHO, ACET, GLY, and MGLY on surface-modified activated carbons are reported for the first time, guiding appropriate approaches to improving indoor air quality.