A strategy is presented for the efficient extraction of hydrocarbons from concrete to enable their monitoring. Both polar and non-polar solvents were examined with the application of several techniques: cold solvent extraction with shaking, Soxhlet, and ultrasound-assisted extraction. The impacts of sample aging and inundation with water on the extraction efficiency were investigated to elucidate the nature of analyte-matrix interactions. Organic matrix-destructive solvents that partially disintegrate concrete (ethyl acetate, methanol, and acetonitrile) were most efficient for all considered scenarios, yielding recoveries in a range of 95-100% upon a two-step, four-day, cold solvent extraction or 24-h Soxhlet extraction even for highly contaminated and aged samples.