title: Application of integrated comprehensive/multidimensional gas chromatography with mass spectrometry and olfactometry for aroma analysis in wine and coffee.
abstract: Component coelution in chromatographic analysis complicates identification and attribution of individual odour-active volatile molecules in complex multi-component samples. An integrated system incorporating comprehensive two-dimensional gas chromatography (GC × GC) and multidimensional gas chromatography (MDGC), with flame ionisation, olfactometry and mass spectrometry detection was developed to circumvent data correlation across different systems. Identification of potent odorants in Shiraz wine and the headspace of ground coffee are demonstrated as selected applications. Multiple solid-phase microextraction (SPME) sampling with GC-O located odour-active regions; GC × GC established the complexity of odour-active regions; MDGC provided high-resolution separation for each region; simultaneous 'O' and MS detection completed the analysis for target resolved peaks. Seven odour regions in Shiraz were analysed with MDGC-O/MS detection, revealing 11 odour volatiles through matching of mass spectrometry and retention indices from both separating dimensions, including acetic acid; octen-3-ol; ethyl octanoate; methyl-2-oxo-nonanoate; butanoic acid, 2-methylbutanoic acid, and 3-methylbutanoic acid; 3-(methylthio)-1-propanol; hexanoic acid; β-damascenone; and ethyl-3-phenylpropanoate. A capsicum odour in ground coffee was identified as 2-methoxy-3-isobutylpyrazine with a 5-fold increase in S/N of the odorant when acquired using a 6-time cumulative SPME sampling approach.
authors.affiliation: Australian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton, VIC 3800, Australia.
authors.forename: Sung-Tong
authors.initials: ST
authors.lastname: Chin
authors.affiliation: Department of Food Science, University of Otago, PO Box 56, Dunedin 9056, New Zealand.
authors.forename: Graham T
authors.initials: GT
authors.lastname: Eyres
authors.affiliation: Australian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton, VIC 3800, Australia. Electronic address: Philip.Marriott@monash.edu.
authors.forename: Philip J
authors.initials: PJ
authors.lastname: Marriott
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D003069:Coffee / Q000737:chemistry*; D006801:Humans; D013058:Mass Spectrometry; D009812:Odorants / Q000032:analysis*; D064367:Olfactometry / Q000379:methods*; D052617:Solid Phase Microextraction / Q000379:methods; D014920:Wine / Q000032:analysis*
chemical_list: D003069:Coffee
keywords: Cryogenic trapping; Cumulative SPME; High resolution GC; Multiple headspace sampling; Odour assessment; Olfactometry; Shiraz wine aroma