This dataset includes raw and processed data demonstrating the use of a new rapid workflow for estimating the biological sex of human individuals using liquid atmospheric-pressure matrix-assisted laser desorption/ionisation (LAP-MALDI) mass spectrometry (MS) and MS/MS analysis of amelogenin peptides. By applying a straightforward classification rule that leverages a panel of MS and MS/MS ion signals, it was also possible to estimate the biological sex of deciduous teeth.

All teeth were obtained from a single site (St. Oswald’s Priory, Gloucester, UK) and together with their skeletal remains curated by the Department of Archaeology at the University of Reading.

All MS and MS/MS analyses were conducted using a modified Synapt G2-Si (Waters, Wilmslow, UK) equipped with a custom-built atmospheric pressure MALDI source.
Raw data were processed with Mascot Distiller (Version 2.8.5.0, 64-bit; Matrix Science, London, UK) for automated peak picking, with each raw data file analysed using three different signal-to-noise ratios (S/N): 2, 10, and 50.