Abstract:A method based on headspace solid-phase microextraction (HS-SPME) coupled to chromatography-mass spectrometry (GC-MS) was developed to quantify the volatile flavor compounds in Fujian Monascus vinegar (Yongchun aged vinegar and Yongchun aromatic vinegar). Optimal extraction conditions showed that incubation of 6 mL vinegar (diluted 10-fold) with 1.5?g of sodium chloride, an extraction time of 40?min, an extraction temperature of 50 ℃ using a DVB/CAR/PDMS fiber will give the best extraction. Under these conditions, totally 63 volatile flavor compounds were identified in Fujian Monascus vinegar, including esters (20), alcohols (12), acids (13), aldehydes (7), ketones(5), phenols (2) and others (4). Ethyl acetate, phenylethyl alcohol, benzaldehyde, isobutyl acetate, cedrol, acetoin and acetic acid were the main volatile compounds in Fujian Monascus Vinegar. Isobutyl acetate, 2-acetoxy-3-butanone and heptanoic acid were strongly associated with Yongchun aged vinegar, whereas octanoic acid, 2-dodecanol, butanoic acid, styrene, ethyl hexanoate and 1-nonanol showed statistically significant positive correlations with Yongchun aromatic vinegar.