Total-transfer comprehensive three-dimensional gas chromatography with time-of-flight mass spectrometry.

Autor: Trinklein TJ; Department of Chemistry, Box 351700, University of Washington, Seattle, WA 98195, USA., Schöneich S; Department of Chemistry, Box 351700, University of Washington, Seattle, WA 98195, USA., Sudol PE; Department of Chemistry, Box 351700, University of Washington, Seattle, WA 98195, USA., Warren CG; Department of Chemistry, Box 351700, University of Washington, Seattle, WA 98195, USA., Gough DV; Department of Chemistry, Box 351700, University of Washington, Seattle, WA 98195, USA., Synovec RE; Department of Chemistry, Box 351700, University of Washington, Seattle, WA 98195, USA. Electronic address: synovec@chem.washington.edu.
Jazyk: angličtina
Zdroj: Journal of chromatography. A [J Chromatogr A] 2020 Dec 20; Vol. 1634, pp. 461654. Date of Electronic Publication: 2020 Oct 29.
DOI: 10.1016/j.chroma.2020.461654
Abstrakt: Although comprehensive two-dimensional (2D) gas chromatography (GC × GC) is a powerful technique for complex samples, component overlap remains likely. An intriguing route to address this challenge is to utilize the additional peak capacity and chemical selectivity provided by comprehensive three-dimensional (3D) gas chromatography (GC 3 ), especially with time-of-flight mass spectrometry detection (GC 3 -TOFMS). However, the GC 3 -TOFMS instrumentation reported to date has employed one or both modulators with a duty cycle < 100%, making the potential gain in detection sensitivity over GC × GC modest, or perhaps even worse. Herein, we describe instrumentation for GC 3 -TOFMS in which both modulators provide total-transfer (100% duty cycle). Specifically, the instrument is based on the facile modification of a commercial thermally modulated comprehensive GC × GC-TOFMS platform for modulation from the 1 D column to the 2 D column, with recently described dynamic pressure gradient modulation (DPGM) as the second modulator from the 2 D column to the 3 D column, which is a total-transfer flow modulation technique. Area measurements of 1 D peaks are compared to the sum of 3 D peak areas to validate the assumption that total-transfer from 1 D to 3 D is accomplished. Additionally, peak heights were amplified by as high as a factor of 177 (x̅ = 130, s = 47) via comparison of 1 D peak heights to the maximum 3 D peak heights. Column selection is explored, with emphasis on the resulting peak width-at-base on each dimension and usage of 3D space as evaluation metrics. Using a nonpolar × polar × ionic liquid column combination, an effective peak capacity which considers modulation-induced broadening as high as 32,300 for select analytes was achieved (x̅ = 19,900, s = 10,700). The analytical benefits of employing three selective phases, mass spectrometry detection, and total-transfer modulation are explored with separations of a metabolomics-type sample, i.e., derivatized porcine serum, and a jet fuel spiked with various sulfur-containing compounds.
Competing Interests: Declaration of Competing Interest None.
(Copyright © 2020. Published by Elsevier B.V.)
Databáze: MEDLINE
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