In this study, polyester-based textile fibers were treated with several liquid-solvents and the extracts were spectrometrically characterized. The solvents used were ethanol-ether (1:1), ethanol-HCl (1:1), and carbon tetrachloride. Spectrometric characterization of the extracts included a first study by UV-visible spectrophotometry, fluorescence spectroscopy, and Fourier transform-infrared spectrometry after a liquid chromatographic fractionation. However, final elucidation was carried out by liquid chromatography-mass spectrometry, which provides enough sensitivity, and fast and reproducible results. The organic compounds identified in the extracts were usual additives largely employed in the manufacture of textile fibers. Some of these organic compounds can constitute potential hazards for human health.