In order to analyze the volatile compounds of Daqu after different treatment, the effect of hot-air drying process on the volatile compounds of Daqu in storage period was investigated using headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS)and analyzed by principal component analysis. The results showed that 54 kinds of volatile flavor compounds were detected from all samples, mainly including alcohols, esters, aromatics, pyrazines, alkanes, aldehydes and ketones and heterocycles. The aroma components of daqu after different treatment were significantly different. The first class of principal components included furfuryl alcohol, isoamyl alcohol, 6,10,14-trimethyl-2-pentadecanone, benzaldehyde, 2-n-pentylfuran and ethyl valerate. The second class was the long-chain esters. Moreover, hot-air drying process could increase the contents of alcohols, esters, aromatic and pyrazine of Daqu during storage. The volatile components of Daqu impacted by hot air drying process mainly were explained as long chain esters. Alcohols and alkanes were the special compounds in these Daqu and were different from the others. This study provides a reference for the industrialization of Daqu and exploration of the hot-air drying process.