As part of an ongoing pharmacokinetic investigation of the teratogenicity of phenol and its metabolites (1,2-, 1,3-, and 1,4-dihydroxybenzene) in pregnant Sprague-Dawley rats, there was need of an analytical procedure sufficiently sensitive to provide quantitative data to the parts-per-billion level or better in urine, plasma, and fetal tissue. In the development of an extraction method utilizing the 'salting out' technique, the extraction efficiencies of phenol, catechol, resorcinol, and hydroquinone from aqueous solutions were determined for tetrahydrofuran (THF), acetonitrile (ACN), dimethylformamide (DMF), ethyl acetate (EtOAc), and diethyl ether (Et2O). The inorganic salts of potassium fluoride (anhydrous), sodium chloride, lithium chloride, ammonium acetate, and sodium bicarbonate were used to saturate the solvent/water combinations. Phase separations were not observed for THF/LiCl, NaHCO3; ACN/NaHCO3; and DMF/NaCl, LiCl, NH4OAc, NaHCO3, whereas ACN/KF produced quinone while DMF/KF yielded no hydroquinone in non-acidified solutions. Essentially all other solvent/salt combinations gave quantitative recoveries, while KF was found to be an efficient drying agent.