The aim of this study was to explore the effects of freeze-thaw (FT) cycles on meat quality, myofibrillar protein gelation and emulsification properties, and exudate metabolome changes in pork loins. Meat tenderness improved (P < 0.05), whereas water-holding capacity (WHC), meat color attributes declined (P < 0.05) with FT cycles. Multiple FT accelerated meat lipid and protein oxidations. Decreases in strength and WHC of myofibrillar protein gels with FT cycles were confirmed. Myofibrillar protein emulsions with more FT cycles showed a decrease in the emulsifying activity index (P < 0.001) and larger oil droplets, resulting in poorer storage stability. A total of 501 metabolites were tentatively identified in pork exudates, with 21 metabolites significantly correlated (P < 0.05 and r > 0.6) with meat quality attributes. These results demonstrated the potential of using the metabolomic information from exudates to elaborate on or even predict the FT cycles, or meat quality.