Methyl parathion (MPT; O,O-dimethyl-O-4-nitrophenyl phosphorothioate) and its active metabolite, methyl paraoxon (MPO; O,O-dimethyl-O-4-nitrophenyl phosphate), were isolated from raw milk by solid-phase extraction (SPE) and determined by gas chromatography with flame photometric detection. The SPE method was compared with a traditional liquid-liquid extraction (LLE) procedure to determine whether SPE had suitable sensitivity and better efficiency in extracting MPT and MPO from milk of cows and goats. Method detection limits were higher for SPE, but the differences were not significant (t-test). Recoveries of MPT and MPO from raw milk samples spiked at 0.05, 0.5, and 5.0 micrograms/mL ranged from 80.0 to 118%, and the coefficients of variation were usually less than 10% for both methods. LLE required more organic solvents and was more time consuming compared with SPE.