A method for pretreating and extracting a liquid sample by sorbing an aqueous liquid sample, including an organic analyte and an acid or a base, in a solid sorbent material, and at least partially neutralizing the acid or base by reaction with neutralizing ions retained on a support surface, and contacting the liquid sample-sorbed sorbent material at elevated temperature and pressure with an organic solvent to extract the analyte into said solvent, preferably in a vessel having an extraction chamber with a zirconium metal interior surface.