Malodors in wastewater from animal-rearing facilities are due to the presence of characteristic polar compounds. The efficiency and reproducibility of three solid-phase microextraction (SPME) fibers (Carboxen-PDMS, polyacrylate, and PDMS) as well as PDMS-coated stir bars for the measurement of some of these compounds in the liquid phase were compared. In initial experiments, the SPME fibers and stir bars were exposed to a standard water solution containing a mixture of 18 compounds with a range of octanol-water partition coefficients. The polyacrylate SPME fibers and PDMS-coated stir bars, having been found to possess the best combination of extraction efficiency and reproducibility of measurement, were compared for the extraction of a high-strength swine wastewater. Ten compounds, which are known contributors to malodors in wastewater, were quantified by both methods of extraction. For most compounds, greater levels were estimated by the PDMS-coated stir bars than by SPME, and measurement reproducibility was also greater. For both methods of extraction, there was greater variation in the measurement of volatile fatty acids than there was for aromatics.