| Summary: | In this paper, the differentiation of three ripening stages, postsalting, drying, and cellar, of Iberian dry-cured ham has been carried out according to their free amino acids contents. Eighteen L-amino acids, alanine, 2-aminobutanoic acid, aspartic acid, cysteine, glutamine, glycine, histidine, hydroxyproline, isoleucine, leucine, lysine, methionine, phenylalanine, proline, serine, threonine, tyrosine, and valine have been determined by gas chromatography with derivatization with N,O-<i>bis</i>(trimethylsilyl)-trifluoroacetamide. Gas chromatography−mass spectrometry was used to confirm the presence of the eighteen amino acids in the ham samples, and gas chromatography using a DB-17HT column and flame ionization detector was used for quantitative determination. Extraction with a mixture methanol-acetonitrile has been carried out, achieving recoveries in the range 52−164%. Methimazole was used as internal standard. Limits of detection ranged between 7.0 and 611.7 mg·kg<sup>−1</sup>. Free amino acids have been used as chemical descriptors to differentiate between the ripening stages. Principal component analysis and linear discriminant analysis have been used as chemometric techniques, achieving complete differentiation between the ripening stages. Alanine, tyrosine, glutamine, proline, 2-aminobutanoic acid, cysteine, and valine were the most differentiating amino acids.
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