Abstract: The combined technology of solid phase microextraction(SPME)and gas chromatography-mass spectrometry(GC-MS)was used to analyze the volatile compounds from human breast milk and the detection conditions were optimized by single factor experiments. The optimal conditions were achieved when 5 mL of sample containing 1.5 gram of NaCl was extracted at 60 ℃ for 30 min using DVB/PDMS extraction fiber with a resolution time of 5 min. Under optimal conditions,thirty-four volatile compounds including alkenes(fourteen types),acids(five types),esters(eight types),aromatic hydrocarbons(four types)and ketones(three types)were identified. This study could provide theoretical basis for the improvement of flavor of formula milk.