A passive sampling method, using retracted solid-phase microextraction (SPME) – gas chromatography–mass spectrometry and time-weighted averaging, was developed and validated for tracking marker volatile organic compounds (VOCs) emitted during aerobic digestion of biohazardous animal tissue. The retracted SPME configuration protects the fragile fiber from buffeting by the process gas stream, and it requires less equipment and is potentially more biosecure than conventional active sampling methods. VOC concentrations predicted via a model based on Fick’s first law of diffusion were within 6.6–12.3% of experimentally controlled values after accounting for VOC adsorption to the SPME fiber housing. Method detection limits for five marker VOCs ranged from 0.70 to 8.44 ppbv and were statistically equivalent (p > 0.05) to those for active sorbent-tube-based sampling. The sampling time of 30 min and fiber retraction of 5 mm were found to be optimal for the tissue digestion process.