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Multiple component isolation in preparative multidimensional gas chromatography with characterisation by mass spectrometry and nuclear magnetic resonance spectroscopy
Authors:Christian Rü  hle,Graham T. Eyres,Sylvia Urban,Jean-Pierre Dufour,Paul D. Morrison,Philip J. Marriott
Affiliation:1. Australian Centre for Research on Separation Science (ACROSS), School of Applied Sciences, RMIT University, GPO Box 2476V, Melbourne 3001, Australia;2. Marine and Terrestrial Natural Product (MATNAP) Research Group, School of Applied Sciences, RMIT University, GPO Box 2476V, Melbourne 3001 Australia;3. Department of Food Science, University of Otago, PO Box 56, Dunedin 9054, New Zealand
Abstract:The preparative scale isolation of multiple components from an essential oil matrix is described using multidimensional gas chromatography (prep-MDGC) which allows their further characterisation by mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy. Menthol, linalyl acetate, carvone and geraniol were isolated individually, and were also collected in various combinations. It was demonstrated to be possible to collect multiple selected components from numerous repeat injections of the sample, to permit increased mass recovery from an external cryotrap collection device. Peak retention times remained reproducible (<0.3 s) over the repeated injections and switching events. This methodology may be utilised to confirm peak identity or to produce unique mixed-component reference standards, for instance to allow their identification in other samples using GC/MS, or identify them in comprehensive two-dimensional gas chromatography (GC × GC) analysis.
Keywords:Multidimensional gas chromatography (MDGC)   Nuclear magnetic resonance (NMR) spectroscopy   Gas chromatography&ndash  mass spectrometry (GC/MS)   Cryogenic isolation   Reference standards   Preparative capillary gas chromatography   Essential oil
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