Polymethoxylated flavones (PMFs) were extracted from Pericarpium Citri Reticulatae Viride using a procedure that obtained a consistent mixture of PMFs both in identity and proportion. The mixture consisted of isosinensetin (0.2%) (1), sinensetin (1.7%) (4), tetramethyl-o-isoscutellarein (0.3%) (5), nobiletin (40.5%) (6), tetramethyl-o-scutellarein (1.2%) (7), tangeretin (45.6%) (10), 5-demethylnobiletin (8.7%) (12), 5-demethyl tangeretin (0.8%) (14) and other flavonoids including heptamethoxyflavone (1.0%) (9), among which, compounds 1, 4, 5, 7 and 9 were identified based on their UV spectra, MS data and elution order described in the literature while compounds 6, 10, 12 and 14 were isolated and identified by UV, IR, MS, H-1 NMR, C-13 NMR and 2D NMR spectral studies. In addition, compound 14 was isolated and identified for the first time from Citrus. (c) 2007 Elsevier B.V. All rights reserved.