Abstract: Total volatile basic nitrogen(TVB-N)was used to evaluate the freshness of Thamnaconus modestusas raw muscle under 4℃ in 7 d. Free amino acids,nucleotides and glyoxal were determinated to investigate the effect of fish freshness on the formation of advanced glycation end-products(AGEs)in grilled fish fillets. Overall,the content of free amino acids,nucleotides in both raw muscle and grilled fish fillets,and also total AGEs,Nε-carboxymethyl-lysine(CML),fluorescent AGEs and pentosans in grilled fish fillets increased with the decline of fish freshness,indicating that the freshness of raw muscle was quite relevant to the formation of AGEs in grilled fish fillets.Content of total AGEs and CML were up to 7.24 and 4.01 μg/g,respectively. As a kind of early and middle stage glycosylation products,the content of glyoxal did not change too much in raw muscle within 7 d but increased in grilled fish fillets,indicating that there was a direct connection between the processing of grilled fish fillet and glycosylation reaction.