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Separations
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Two-Dimensional Gas Chromatography
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Two-Dimensional Gas Chromatography

A special issue of Separations (ISSN 2297-8739).

Deadline for manuscript submissions: closed (30 April 2016) | Viewed by 27594

Special Issue Editor

Prof. Dr. Shari Forbes

E-Mail Website
Guest Editor
Centre for Forensic Science, University of Technology, Sydney, PO Box 123, Broadway, NSW 2007, Australia
Interests: decomposition chemistry; volatile organic compounds; two-dimensional gas chromatography

Special Issue Information

Dear Colleagues,

Over the past decade, comprehensive two-dimensional gas chromatography (GC×GC) has become a well-established and valuable technique for separating and analysing complex mixtures. GC×GC has been applied in many fields where conventional one-dimensional (1D) separations were traditionally used for volatile and semi-volatile analysis, including flavour and fragrance, environmental studies, metabolomics, pharmaceuticals, petroleum products, and forensic science. Compared to 1D GC, GC×GC provides enhanced sensitivity and superior separation power due to increased peak capacity. An additional dimension of information can be added by employing detection systems such as time-of-flight mass spectrometers (TOFMS). The ongoing evolution of GC×GC has included advances in modulation, data handling and application development. Improved quantitative data analysis is necessary to move the use of GC×GC from research laboratories to more widespread use in commercial laboratories. Discussion at recent scientific meetings has focused on reaching a near-theoretical peak capacity and the implementation of high resolution TOFMS. This Special Issue invites contributions that highlight the latest research and advancements in GC×GC technology, and demonstrate the range of applications and fields for which its use is particularly beneficial.

Prof. Dr. Shari Forbes
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Separations is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.


Keywords

  • multidimensional chromatography
  • GC×GC
  • HRTOFMS
  • complex mixture characterisation
  • non-targeted analysis
  • chemometrics
  • data handling strategies/software
  • chromatographic alignment
  • peak capacity
  • biomarker discovery
  • application development

Published Papers (5 papers)

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Research

4385 KiB  
Article
Achieving a Near-Theoretical Maximum in Peak Capacity Gain for the Forensic Analysis of Ignitable Liquids Using GC×GC-TOFMS
by Katie D. Nizio, Jack W. Cochran and Shari L. Forbes
Separations 2016, 3(3), 26; https://doi.org/10.3390/separations3030026 - 01 Sep 2016
Cited by 26 | Viewed by 6428
Abstract
At present, gas chromatography–quadrupole mass spectrometry (GC-qMS) is considered the gold standard amongst analytical techniques for fire debris analysis in forensic laboratories worldwide, specifically for the detection and classification of ignitable liquids. Due to the highly complex and unpredictable nature of fire debris, [...] Read more.
At present, gas chromatography–quadrupole mass spectrometry (GC-qMS) is considered the gold standard amongst analytical techniques for fire debris analysis in forensic laboratories worldwide, specifically for the detection and classification of ignitable liquids. Due to the highly complex and unpredictable nature of fire debris, traditional one-dimensional GC-qMS often produces chromatograms that display an unresolved complex mixture containing only trace levels of the ignitable liquid among numerous background pyrolysis products that interfere with pattern recognition necessary to verify the presence and identification of the ignitable liquid. To combat these challenges, this study presents a method optimized to achieve a near-theoretical maximum in peak capacity gain using comprehensive two-dimensional gas chromatography (GC×GC) coupled to time-of-flight mass spectrometry (TOFMS) for the forensic analysis of petroleum-based ignitable liquids. An overall peak capacity gain of ~9.3 was achieved, which is only ~17% below the system’s theoretical maximum of ~11.2. In addition, through the preservation of efficient separation in the first dimension and optimal stationary phase selection in the second dimension, the presented method demonstrated improved resolution, enhanced sensitivity, increased peak detectability and structured chromatograms well-suited for the rapid classification of ignitable liquids. As a result, the method generated extremely detailed fingerprints of petroleum-based ignitable liquids including gasoline, kerosene, mineral spirits and diesel fuel. The resultant data was also shown to be amenable to chromatographic alignment and multivariate statistical analysis for future evaluation of chemometric models for the rapid, objective and automated classification of ignitable liquids in fire debris extracts. Full article
(This article belongs to the Special Issue Two-Dimensional Gas Chromatography)
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2506 KiB  
Communication
Postmortem Internal Gas Reservoir Monitoring Using GC×GC-HRTOF-MS
by Pierre-Hugues Stefanuto, Katelynn A. Perrault, Silke Grabherr, Vincent Varlet and Jean-François Focant
Separations 2016, 3(3), 24; https://doi.org/10.3390/separations3030024 - 17 Aug 2016
Cited by 19 | Viewed by 5035
Abstract
Forensic investigations often require postmortem examination of a body. However, the collection of evidence during autopsy is often destructive, meaning that the body can no longer be examined in its original state. In order to obtain an internal image of the body, whole [...] Read more.
Forensic investigations often require postmortem examination of a body. However, the collection of evidence during autopsy is often destructive, meaning that the body can no longer be examined in its original state. In order to obtain an internal image of the body, whole body postmortem computed tomography (PMCT) has proven to be a valuable non-destructive tool and is currently used in medicolegal centers. PMCT can also be used to visually locate gas reservoirs inside a cadaver, which upon analysis can provide useful information regarding very volatile compounds that are produced after death. However, the non-targeted profiling of all potential volatile organic compounds (VOCs) present in these reservoirs has never been attempted. The aim of this study was to investigate the VOC profile of these reservoirs and to evaluate potential uses of such information to document circumstances surrounding death, cause of death and body taphonomy. Comprehensive two-dimensional gas chromatography coupled to time-of-flight high-resolution mass spectrometry (GC×GC-HRTOF-MS) was used for VOC measurements. This study demonstrated that the chemical composition of VOCs within the gas reservoirs differed between locations within a single body but also between individuals. In the future, this work could be expanded to investigate a novel, non-destructive cadaver screening approach prior to full autopsy procedures. Full article
(This article belongs to the Special Issue Two-Dimensional Gas Chromatography)
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1781 KiB  
Article
Development of a Combined Heart-Cut and Comprehensive Two-Dimensional Gas Chromatography System to Extend the Carbon Range of Volatile Organic Compounds Analysis in a Single Instrument
by Rachel E Dunmore, James R Hopkins, Richard T Lidster, Mohammed Iqbal Mead, Brian J Bandy, Grant Forster, David E Oram, William T Sturges, Siew-Moi Phang, Azizan Abu Samah and Jacqueline F Hamilton
Separations 2016, 3(3), 21; https://doi.org/10.3390/separations3030021 - 20 Jul 2016
Cited by 5 | Viewed by 5945
Abstract
The majority of atmospheric measurements of volatile organic compounds (VOCs) are usually limited to a small range, either in volatility or time resolution. A combined heart-cut gas chromatography (GC) with comprehensive two-dimensional GC (GC×GC) instrument was developed, specifically to increase the number of [...] Read more.
The majority of atmospheric measurements of volatile organic compounds (VOCs) are usually limited to a small range, either in volatility or time resolution. A combined heart-cut gas chromatography (GC) with comprehensive two-dimensional GC (GC×GC) instrument was developed, specifically to increase the number of VOCs analysed using a single instrument. The system uses valve based modulation and was fully automated, making it suitable for use in the field. A laboratory comparison to an existing dual-channel GC (DC-GC) instrument demonstrated that this new GC-GC×GC can accurately measure atmospheric mixing ratios of C 5 -C 13 VOC species with a wide range of functionalities. Approximately hourly field measurements were conducted at a remote marine atmospheric research station in Bachok, Malaysia. This region was shown to be influenced by clean marine air masses, local anthropogenic and biogenic emission sources and aged emissions transported from highly polluted South East Asian regions. A dramatic shift in air mass direction was observed each day associated with the development of a sea breeze, which influenced the diurnal profiles of species measured at the Bachok site. A proton-transfer-reaction mass spectrometer (PTR-MS) was also deployed at Bachok and compared to the new GC-GC×GC instrument. Overall, the GC-GC×GC instrument has been shown to perform well in lab comparisons and during field observations. This represents a good compromise between volatility and high complexity o n l i n e measurements of VOCs. Full article
(This article belongs to the Special Issue Two-Dimensional Gas Chromatography)
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2615 KiB  
Article
GC×GC-TOFMS for the Analysis of Metabolites Produced by Termites (Reticulitermes flavipes) Bred on Different Carbon Sources
by Catherine Brasseur, Julien Bauwens, Cédric Tarayre, Catherine Millet, Christel Mattéotti, Philippe Thonart, Jacqueline Destain, Frédéric Francis, Eric Haubruge, Daniel Portetelle, Micheline Vandenbol, Edwin De Pauw and Jean-François Focant
Separations 2016, 3(2), 19; https://doi.org/10.3390/separations3020019 - 13 Jun 2016
Cited by 1 | Viewed by 3911
Abstract
More and more studies are dedicated to termites and their symbionts, to better understand how they efficiently produce energy from lignocellulose. In that context, a powerful analytical method was developed to perform the detection, separation and identification of compounds in the 1 µL [...] Read more.
More and more studies are dedicated to termites and their symbionts, to better understand how they efficiently produce energy from lignocellulose. In that context, a powerful analytical method was developed to perform the detection, separation and identification of compounds in the 1 µL fluid volume of the gut of the termite Reticulitermes flavipes. Comprehensive two-dimensional gas chromatography (GC×GC) coupled to time-of-flight mass spectrometry (TOFMS) was tested with three different column combinations: (1) low-polar/mid-polar; (2) polar/low-polar and (3) mid-polar/low-polar. The column set (3) offered the best separation and was chosen for further analysis and comparison study. Metabolites were detected in the samples, including amino acids, sugars, amines and organic acids. Samples collected from termites fed for 30 days on Avicel cellulose or xylan powder diets were analyzed and compared with the wood diet. Principal component analysis (PCA) of metabolite profiles demonstrated a separation of different clusters corresponding to the three different diets, with a similar trend for diets containing cellulose. The Analysis of variance (ANOVA) (one way-ANOVA and Tukey’s test) was used to compare compound levels between these three different diets. Significant differences were observed, including higher levels of aromatic derivatives in the wood diet and higher levels of sugar alcohols in the xylan diet. A higher accumulation of uric acid was observed with the artificial diets (cellulose and xylan), likely to be related to the nitrogen deficiency. The present study highlighted the capability of adaptation of the termite system to non-optimal carbon sources and the subsequent modification of the metabolite profile. These results demonstrate the potential interest to investigate metabolite profiling with state-of-the-art separation science tools, in order to extract information that could be integrated with other omics data to provide more insight into the termite-symbiont digestion system. Full article
(This article belongs to the Special Issue Two-Dimensional Gas Chromatography)
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5620 KiB  
Communication
A New Approach for the Characterization of Organic Residues from Stone Tools Using GC×GC-TOFMS
by Katelynn A. Perrault, Pierre-Hugues Stefanuto, Lena Dubois, Dries Cnuts, Veerle Rots and Jean-François Focant
Separations 2016, 3(2), 16; https://doi.org/10.3390/separations3020016 - 18 May 2016
Cited by 16 | Viewed by 5630
Abstract
Headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) have traditionally been used, in combination with other analyses, for the chemical characterization of organic residues recovered from archaeological specimens. Recently in many life science fields, comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) has [...] Read more.
Headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) have traditionally been used, in combination with other analyses, for the chemical characterization of organic residues recovered from archaeological specimens. Recently in many life science fields, comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) has provided numerous benefits over GC-MS. This study represents the first use of HS-SPME-GC×GC-TOFMS to characterize specimens from an experimental modern reference collection. Solvent extractions and direct analyses were performed on materials such as ivory, bone, antlers, animal tissue, human tissue, sediment, and resin. Thicker film column sets were preferred due to reduced column overloading. The samples analyzed by HS-SPME directly on a specimen appeared to give unique signatures and generally produced a higher response than for the solvent-extracted residues. A non-destructive screening approach of specimens may, therefore, be possible. Resin and beeswax mixtures prepared by heating for different lengths of time appeared to provide distinctly different volatile signatures, suggesting that GC×GC-TOFMS may be capable of differentiating alterations to resin in future studies. Further development of GC×GC-TOFMS methods for archaeological applications will provide a valuable tool to uncover significant information on prehistoric technological changes and cultural behavior. Full article
(This article belongs to the Special Issue Two-Dimensional Gas Chromatography)
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