A method for the determination of volatile compounds from Colla Corii Asini by headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrome-try(GC-MS) combined with AMDIS was established.The total peak area and number of peaks of the volatile compounds were used as indices to optimize the different extraction conditions by single factor and orthogonal test. The results showed that the influence of extraction temperature was larger. The better extraction conditions were: the sample amount of 5 g, equilibration time 10 min, extracted for 50 min at 70 ℃ by 50/30 μm DVB/CAR/PDMS fiber and then desorbed 5 min. Under these conditions, 41 species of volatile components from Colla Corii Asini were identified, including 10 pyrazines, 8 aldehydes, 5 esters, 6 ketones and 13 others. Among of these, the higher relative contents were pyrazines and aldehydes, accounting for 48.95% and 26.37% of the total components, respectively.The average RSD of the peak area of volatile compounds was 6.25%，which showed that the repeatability of the method was well.This method provides a theoretical basis for the quality control and product research and development of Colla Corii Asini.