Head Space Solid phase micro-extraction(HS/SPME) coupled with gas chromatography(GC) were used for the determination of volatile compounds in goat milk. HS/SPME experimental parameters, such as SPME fibre, extraction temperature, NaCl concentration, extraction time and desorption time were optimized using the number and area of peaks as index. The optimal extraction efficiency for goat milk was achieved when sample was headed at 70 ℃ for 90 min after the addition of 0.3 g/mL NaCl, extracted by a carboxen/polydimethylsiloxane(CAR/PDMS) fibre, and than the fibre was transferred to a GC injection port for thermal desorption at 250 ℃ for 5 min. As a result, 42 kinds of volatile components were detected that including acids(14 kinds), esters(6 kinds), hydrocarbons(5 kinds), alcohols(4 kinds), aldehydes(3 kind), aromatic(5 kinds) and heterocyclic(5 kinds).
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