Geosmin (GSM) and 2-methylisoborneol (MIB) are naturally occurring volatile organic compounds derived from microbial metabolism. Relatively low concentrations of GSM and MIB can concentrate from water into fish tissues, imparting an earthy and unpleasant flavor. Previous analytical methods focused on detection of GSM and MIB in water because extraction from fish tissue is complicated by the lipid-rich matrix. A method was developed at the University of Maine’s Aquaculture Research Institute (ARI) for the extraction and detection of MIB and GSM from fish using a robust metal probe bearing a high-capacity sorptive extraction phase (HiSorbTM) containing polydimethylsiloxane (PDMS), carbon wide range (CWR), and divinylbenzene (DVB). This method out-performs other extraction techniques by allowing for full automation, improved throughput, and a reduction in laboratory preparation errors. Robust and quantitative detection limits were achieved even with complex fish tissue matrixes using an internal standard, a matrix match calibration curve, and an increased extraction temperature and time. This method detects GSM and MIB below human tasting thresholds making it suitable for evaluating product quality in aquaculture. This method can be implemented to extract GSM and MIB from various other organ tissues as well, increasing its applicability for researchers and aquaculture farmers.