Three polymethoxyflavonoids (PMFs) from citrus peel: tangeretin (TG), isosinensetin (ISN), and 3',4',5,7-tetramethoxyflavone (TMHF) and their combination significantly inhibited heterocyclic amines (HAs) and advanced glycation-end products (AGEs) formation. In particular, ISN with five methoxyl structure and B-ring distribution was significantly effective reduce HAs to 50.1 %-77.9 %. The PMF mixture was effective reduce both HAs and AGEs at rates of 52.2 %-77.3 % and 16.4 %-66.8 %, respectively. For ISN, the radical scavenging activity and inhibitory effects of HAs and AGEs were highly correlated. However, the inhibitory action of mixed PMFs against harmful substances was related to free radical scavenging activity and their impact on water distribution. Furthermore, GC-IMS analysis revealed the PMF mixture did not significantly change the key aldehyde and ketone compounds in grilled meat. This study provides insights into the effect of PMF mixtures, which appear to synergistically regulate the formation of aromatic and harmful compounds in grilled meat products.