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An analytical method for detecting flame retardants was slightly modified and optimized for the simultaneous determination of 11 organophosphate esters (OPEs) and 26 polyfluoralkyl substances (PFASs) contained in dust. All the analytes were determined in HPLC/MS-MS, and OPEs were also analyzed in GC/MS, and the results were compared. The study was conducted through the investigation of the Standard Reference Material SRM 2585 of the National Institute of Standard and Technology (NIST). The results were compared with the available reference mass fraction reported in the NIST certificate. The mass fraction obtained for the other OPEs and PFASs was compared to available data in the literature. After verifying the reliability of the results, the method was applied to environmental samples of settled dust, collected in four workplaces, where OPE and PFAS content is expected to be higher than in house dust: a mechanical workshop, an electronic repair center, a disassembly site, and a shredding site of two electronic waste recycling plants. By analyzing both PFASs and OPEs in the same samples, the present work demonstrated that the selected working places were more polluted in OPEs than houses; on the contrary, PFAS content in house dust proved to be more than ten times higher than that in workplaces. Additional research is necessary to confirm these data. Nevertheless, because this preliminary study showed not negligible concentrations of OPEs in some workplaces and of PFASs in houses, their monitoring should be extended to other domestic and selected working sites., (© 2022. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)