Several freshness and spoilage indicators were monitored to characterize the postmortem biochemistry of giant squid (Dosidicus gigas) mantle muscle. Squid samples were obtained directly from the sea and kept at 0 °C during a 15-d storage period. Data at zero time were obtained from cryogenically frozen samples at time of capture. The adenosine 5'-triphosphate (ATP) degradation followed a different pattern as compared with that from fish species. ATP was almost completely depleted at 24-h postcatch from 6.54 to <1 μmol/g, while at the same time Hx was the predominant catabolite with a concentration of 4 μmol/g, reaching 6.85 μmol/g at day 15. K-value data followed a logarithmic pattern with time instead of a linear one, with no change after day 3, thus reducing its suitability as a freshness index. The coefficient Hx/AMP seems to be an adequate alternative for this purpose due to its constant increment with time. The high NH4Cl content in mantle muscle (461.3 ± 24.5 mg of NH4+/100 g) derived from its physiological importance for the species compromises the use of the distillation step of the TVB-N analysis commonly used as a spoilage index. This fact explains why the initially high value of TVB-N detected in mantle muscle (243.7 mg N/100 g) did not correlate with the initial low TMA-N content (1.5 ± 0.1 mg/100 g of muscle). The results suggested that under the experimental conditions the shelf life of squid exceeds 15 d. © 2007 Institute of Food Technologists.