To investigate the chemical constituents and anti-inflammatory activity of Cinnamomi Camphorae Radix, various chromatographic separation methods were employed to isolate and purify the chemical components. The structures of compounds were identified based on their physicochemical properties, spectroscopic data, and literature reports, and their anti-inflammatory activities were evaluated using lipopolysaccharide (LPS)-induced RAW 264.7 cell inflammation model. Seventeen compounds were identified as 3,7-dimethyl-oct-1-ene-3,6,7-triol (1), 1α,2β,4β-trihydroxy-p-menthane (2), 1-hydroxy-4-(2-hydroxypropan-2-yl)-1-methylcyclohex-3-en-2-one (3), 2-exo-hydroxycineole (4), 2,3,6,7,10-pentaol (5), 9-oxo-nerolidol (6), 3,7,11-trimethyl-1,7(E),10-dodecatriene-3-ol-9-one (7), 1β,6α-dihydroxy-4(14)-eudesmene (8), (1S,2S)-1,2,3-trihydroxy-1-(3,4-methylenedioxyphenyl) propane (9), 3,4-methylenedioxycinnamyl alcohol (10), quercetin (11), naringenin (12), calamusin I (13), pinnatolide (14), 9β-hydroxysesamin (15), 2-(3,4-methylenedioxyphenyl)-1,2-ethanediol (16), and bis(2-ethylhexyl) terephthalate (17). Among these, compounds 2, 3, 5, 8, 9, 10, 13, 14, 16, and 17 were isolated from Cinnamomum camphora (L.) J. Presl for the first time. Compounds 1, 5, and 11 exhibited inhibitory effects on NO release in LPS-induced RAW 264.7 cells and demonstrated no cytotoxicity. Notably, compound 11 exhibited the most potent inhibition, with an IC₅₀ value of 39.5 ± 4.4 μmol/L, which is comparable to that of the positive control indomethacin (34.2 ± 5.7 μmol/L).