<p>Plastic straws have led to environmental concerns due to their limited reusability and poor recyclability. In response, alternative straws made from materials such as paper, polylactic acid (PLA), and bamboo have been introduced as sustainable options. However, the chemical safety of these alternatives, particularly regarding per- and polyfluoroalkyl substances (PFAS), remains unclear. This study investigated the occurrence of PFAS and other potentially hazardous compounds in disposable straws marketed in Korea. A total of 64 straw samples representing various materials were analyzed. Quantitative analysis of 33 PFAS compounds was conducted using liquid chromatography–tandem mass spectrometry (LC–MS/MS), and suspect screening was performed using ultra-high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (UHPLC-QTOF). Among the 33 PFAS, 16 compounds were detected above the limit of detection. Paper straws exhibited the widest variety and highest concentrations of PFAS, including perfluorooctanoic acid (PFOA) and perfluorobutanoic acid (PFBA). Several precursor compounds with potential for environmental transformation were detected exclusively in paper straws. PFAS concentrations significantly differed by material, with higher levels in paper straws than in plastic and PLA (<i>p</i> &lt; 0.05). In the suspect screening, dioctyl phthalate (DOP) and oleamide were tentatively identified in two paper straw. However, due to the limited sample size and lack of standard confirmation, these findings should be interpreted cautiously. Although paper straws are promoted as environmentally friendly, they may still pose chemical risks to human health. Further studies are needed to assess migration, exposure risks, and inform future regulatory and consumer safety efforts.</p>