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An analytical method using gas chromatography isotope ratio mass spectrometry (GC-IRMS) combined with solid phase micro-extraction (SPME) was developed to measure the δ 13C values of six typical volatiles commonly occurring in wine (isoamyl acetate, 2-octanone, limonene, 2-phenylethanol, ethyl octanoate and ethyl decanoate) for the first time. SPME selected with a divinylbenzene/carboxen/polydimethylsiloxane fiber was combined with the GC-IRMS for pretreatment optimization. The optimized SPME parameters of extraction time, extraction temperature and salt concentration were 40 min, 40 °C and 10%, respectively. The δ 13C values measured by SPME-GC-IRMS were in good agreement with those measured via elemental analyzer (EA)-IRMS and GC-IRMS. The differences range from 0.02 to 0.44‰ with EA-IRMS and from 0 to 0.28‰ with GC-IRMS, indicating the high accuracy of the method. This newly established method measured the precision within 0.30‰ and was successfully validated to discriminate imported real wine samples with identical label but amazing price differences from different importers. [ABSTRACT FROM AUTHOR]