Cancer is a leading cause of fire service morbidity and mortality [1,2]. During a fire, firefighters are exposed to smoke and elevated levels of organic chemicals, such as flame retardants, originating from furniture, carpets, and so forth, as well as their combustion by-products. A high-resolution MS used in full spectrum acquisition mode is extremely advantageous for the untargeted analysis of the environmental contaminants in complex matrices, especially for identification of trace compounds. To identify polycyclic aromatic hydrocarbons (PAHs) and polybrominated diphenyl ethers (PBDEs) and other combustion products, we used a novel high-resolution Agilent 7250 GC/Q-TOF.