The volatile compounds of Yueshengzhai fragrant beef were extracted by solid phase microextraction with three different solid phase microextraction fibers：65um PDMS/DVB，75um CAR/PDMS and 50/30um DVB/CAR/PDMS. Volatile compounds were identified by gas chromatography-mass spectrometry. Comparison the difference of volatile compounds extracted with different solid phase microextraction fibers, and then found the fit solid phase microextraction fiber. 53 volatile compounds were extracted by them. Comparison with the extracted outcome, 75um CAR/PDMS was the best solid phase microextraction fibers for extracting volatile compounds of Yueshengzhai fragrant beef.