The sex profile estimation of pre-historic communities is often complicated by the commingled and scattered nature of skeletal assemblages. Demographic profiles are usually lacking and provide very truncated representations of these populations but proteomic analysis of sex-specific amelogenin peptides in tooth enamel brings new promise to these studies. The main objective was to obtain the sex profile of the human assemblage recovered from the Neolithic cave-necropolis of Escoural (Montemor-o-Novo, southern Portugal) through liquid chromatography-mass spectrometry. The secondary objective was to analyse sex-specific linear enamel hypoplasias (LEH), and to test the reliability of canine odontometric sex estimation. Sex estimation through peptide analysis was carried out in 36 left permanent canines which were macroscopically examined for the presence of LEH. The canine buccolingual diameter was used for odontometric sex estimation. The obtained sex ratio (0.5:1, M:F) is biased to female individuals, probably due to cultural factors since the natural sex ratio of the human population falls between 0.95:1 and 1.02:1 (M:F). A high frequency of LEH was observed, but with no significant sexual differences (p = 0.554). The mean LEH age of onset occurred at 3 years of age, with no significant differences between the sexes (p = 0.116), and was possibly related to the weaning process. Odontometric sex estimation revealed a correct classification of 80%, with a high number of males mistakenly attributed to females. This study is one of the largest samples subjected to peptide analysis, and thus demonstrates its usefulness on the research of commingled and scattered skeletal assemblages.
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