In this paper, extraction of sauced duck neck meat volatile compounds by solid-phase microextraction (SPME) was optimized. Three extraction temperatures (30, 45, 60°C), three extraction times (15, 30, 45 min), and three different fiber coatings (divinylbenzene/carboxen/polydimethylsiloxa n e ( D V B / C A R / P D M S ) , p o l yd i m eth y l s i l o xa n e/ divinylbenzene (PDMS/DVB), and polydimethylsiloxane (PDMS)) were assayed. There were 82 volatile compounds identified and quantified, which belonged to nine families of chemicals including alcohols, acids, esters, ketones, aldehydes, aromatic compounds, heterocycles, monoterpenes, oxygenated monoterpenes, and sesquiterpenes. The major volatile compounds of sauced duck neck came from spices addition, oxidation, Maillard reaction, etc. Almost all the compounds were extracted by the DVB/CAR/PDMS fiber at 45°C, and the optimal time of extraction in this case was 15 min, during which DVB/CAR/PDMS fiber reached equilibration. Among the fibers tested, DVB/CAR/PDMS fiber favored the extraction of a wide range of compounds with low and high boiling point. On the other hand, PDMS/DVB fiber absorbed more polar and high retention index (RI) aromatic compounds.