The monoterpene hydrocarbons in the headspace of Xiangyuan (Citrus wilsonii Tanaka) juice after debittering treatment by macroporous resin were identified and qualified. Eleven monoterpene hydrocarbons were identified by solid phase micro extraction gas chromatography-mass spectrometry (SPME-GC-MS) and rentation index (RI) which was calculated from n-alkane. Then, eight terpenes (α-Pinene, β-Pinene, β-Myrcene, β-Phellandrene, α-Terpinene, Limonene, γ-Terpinene, α-Terpinolene) were quantified by headspace-gas chromatography-flame ionization detector (HS-GC-FID) using partial external standards method. Results showed that the contents of the eight terpenes after debittering were 90.95, 27.5, 26.22, 8.37, 4.17, 843.46, 107.66 and 4.24 ng/L, respectively, and all values were about one tenth of the control. Moreover, the proportions of the substances were not changed by debittering. the limonene had the highest content, followed by γ-Terpinene.