Abstract: In this paper, a method for the determination of odors from silver carp using headspace solid phase microextraction (HS SPME) and gas chromatography mass spectrometry (GC/MS) was presented. The SPME fiber was coated with polydimesiloxane divinylbenzene (PDMS DVB). The extraction and chromatography conditions were optimized with compared some common analysis in fish meat volatiles. The volatiles were hexanal,1 hexanol, heptanal, heptanol, octanel, 1 octen 3 ol and nonanal. The results showed that SPME was effective to analysis of the volatiles in fish meat.