Gelatines from mackerel (Scomber scombrus) heads were extracted after pre-treatment with different organic acids (acetic, citric, lactic, malic and tartaric acids). The organic acid slightly affected the extraction yield, but not significantly (p>0.05). The amino acid profiling found that glycine, proline and hydroxyproline were the major amino acids present in all extracted gelatines. FTIR and 1 H NMR analyses showed that lactic and tartaric acids degraded the molecular structure of the gelatines. The composition and physicochemical properties were also affected by the organic acid used. Gelatine extracted after pre-treatment with acetic acid showed a significantly (p<0.05) higher b* value than the other gelatines, indicating a yellowish color. The use of lactic acid produced a significant increment in turbidity (176±3.2 FTU), reflecting a lack of clarity. The best quality gelatines, in terms of physicochemical properties, were successfully extracted from mackerel heads after pre-treatment with citric and malic acids.