Liquid-liquid and solid phase extraction methods were developed for the accurate and rapid quantitation of radioactive components in human plasma following injection of two PET ligands. A solid phase extraction (SPE) method was developed for the determination of the 5HT(1A) receptor ligand [N-[2-[4-(2-methoxyphenyl) piperazino]ethyl]-N-(2-pyridinyl) trans-4-[(18)F]fluorocyclohexanecarboxamide (FCWAY), and its acidic metabolite, 4-[(18)F]fluorocyclohexane carboxylic acid (FC). In both cases, the extraction method was much faster and easier to use, yet provided results comparable to HPLC and TLC methods. In addition, an easy to perform two-step liquid-liquid extraction was developed for quantitation of 3-(3-((3-[(18)F]fluoropropyl)thio)-1,2,5-thiadiazol-4-yl)-1,2,5,6-tetrahydro-1-methylpyridine ([(18)F]FP-TZTP), a selective M2 muscarinic agonist.