Charcoal-grilled marinated beef (CMB) is a popular Korean food that has garnered worldwide attention. In this study, volatile and odor-active compounds generated in CMB were analyzed using gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry (GC-O). Solvent-assisted flavor extraction and solid-phase micro extraction were employed to extract the volatile compounds before GC-MS and GC-O analyses. In total, 196 compounds were identified in CMB. Certain heterocyclic compounds, such as pyrazines and thiazoles, could be produced by grilling at high temperatures. The formation of benzene derivatives and phenols could be attributed to charcoal grilling and marinade used. In the GC-O results, 3-methylsulfanylpropanal, 2-methoxyphenol, 1,3-benzothiazole, furaneol, 3-methylphenol, prop-2-ene-1-thiol, 2-ethyl-3,5-dimethylpyrazine, and 2,5-dimethylpyrazine exhibited relatively high flavor dilution factors. Based on these findings, sulfur-containing compounds, pyrazines, phenols, and aldehydes primarily influence the characteristic flavor of CMB.