Polar species in jet fuel, such as phenols, may be responsible for a number of performance characteristics of the fuel. However, because they are present at trace levels in fuels, the isolation and detection of these species is difficult. This work describes the development of a simple extraction method using methanol to remove polar phenolic components from petroleum-derived fuels. The method uses the affinity for polar components in the fuel, such as phenols, to partition into methanol, facilitating their removal by typical liquid-liquid extraction protocols. The method is amenable to large fuel sample volumes, thus minimizing limitations encountered with trace oxygenate concentrations, and has proven to be efficient for the removal of many oxygen-containing compounds, including alcohols, carboxylic acids, and phenols from fuel matrixes. The method has been successfully applied to a variety of phenols and appears to be less susceptible to the environment around the -OH group than other extraction methods. Moderate amounts of alkanes and aromatics are also removed using this extraction method, which may present problems when using certain detection schemes. An adsorption technique based on HPLC with a silica column was developed to further separate the extract into one fraction containing alkanes and aromatics and another fraction containing polar species including phenols. The effectiveness of the methanol extraction and HPLC fractionation method was illustrated by data from spiking studies, which show the removal of oxygenates, even hindered phenols, from spiked solvents, from spiked fuels, and from spiked petroleum-derived fuels (JP-8). The method was used to isolate and identify several phenolic species in petroleum-derived jet fuels.