Volatile flavor compounds in three parts of meat from Yanbian yellow cattle were analyzed by headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). The extraction fibers were optimized by comparison of 65 μm PDMS/DVB, 75 μm CAR/PDMS and 100 μm PDMS. The results showed that 65 μm PDMS/DVB had the best extraction effect on the volatile components of meat from Yanbian yellow cattle. Furthermore, the volatile components in Longissimus dorsi, rump and Sirloin of Yanbian Yellow Cattle were respectively investigated, and the differences of the volatile components in the three parts were analyzed with principal component analysis. The results showed that there were differences on the amounts and types of volatile components and areas of chromatography peaks among the three parts. There was no regularity in categories of volatile components. 155 compounds were extracted from three parts and 15 compounds were common including 6 alcohols, 7 aldehydes, 1 ketone, and 1 other chemical.