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Sequential hybrid three-dimensional gas chromatography with accurate mass spectrometry: a novel tool for high-resolution characterization of multicomponent samples

Citation

Yan, D and Wong, YF and Whittock, SP and Koutoulis, A and Shellie, RA and Marriott, PJ, Sequential hybrid three-dimensional gas chromatography with accurate mass spectrometry: a novel tool for high-resolution characterization of multicomponent samples, Analytical Chemistry, 90, (8) pp. 5264-5271. ISSN 0003-2700 (2018) [Refereed Article]

Copyright Statement

Copyright 2018 American Chemical Society

DOI: doi:10.1021/acs.analchem.8b00142

Abstract

A novel sequential three-dimensional gas chromatography–high-resolution time-of-flight mass spectrometry (3D GC–accTOFMS) approach for profiling secondary metabolites in complex plant extracts is described. This integrated system incorporates a nonpolar first-dimension (1Dnp) separation step, prior to a microfluidic heart-cut (H/C) of a targeted region(s) to a cryogenic trapping device, directly followed by the rapid reinjection of a trapped solute into a polar second-dimension (2DPEG) column for multidimensional separation (GCnp–GCPEG). For additional separation, the effluent from 2DPEG can then be modulated according to a comprehensive 2D GC process (GC×GC), using an ionic liquid phase as a third-dimension (3DIL) column, to produce a sequential GCnp–GCPEG×GCIL separation. Thus, the unresolved or poorly resolved components, or regions that require further separation, can be precisely selected and rapidly transferred for additional separation on 2D or 3D columns, based on the greater separation realized by these steps. The described integrated system can be used in a number of modes, but one useful approach is to target specific classes of compounds for improved resolution. This is demonstrated through the separation and detection of the oxygenated sesquiterpenes in hop (Humulus lupulus L.) essential oil and agarwood (Aquilaria malaccensis) oleoresin. Improved resolution and peak capacity were illustrated through the progressive comparison of the tentatively identified components for GCnp–GCPEG and GCnp–GCPEG×GCIL methods. Relative standard deviations of intraday retentions (1tR, 2tR,, and 3tR) and peak areas of ≤0.01, 0.07, 0.71, and 7.5% were achieved. This analytical approach comprising three GC column selectivities, hyphenated with high-resolution TOFMS detection, should be a valuable adjunct for the improved characterization of complex plant samples, particularly in the area of plant metabolomics.

Item Details

Item Type:Refereed Article
Keywords:hop, gas chromatography
Research Division:Chemical Sciences
Research Group:Analytical Chemistry
Research Field:Analytical Spectrometry
Objective Division:Plant Production and Plant Primary Products
Objective Group:Horticultural Crops
Objective Field:Hops
UTAS Author:Yan, D (Ms Dandan Yan)
UTAS Author:Whittock, SP (Mr Simon Whittock)
UTAS Author:Koutoulis, A (Professor Anthony Koutoulis)
UTAS Author:Shellie, RA (Associate Professor Robert Shellie)
ID Code:129278
Year Published:2018
Funding Support:Australian Research Council (LP140100160)
Web of Science® Times Cited:5
Deposited By:Plant Science
Deposited On:2018-11-20
Last Modified:2019-03-26
Downloads:0

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