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GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition)

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A special issue of Chemosensors (ISSN 2227-9040). This special issue belongs to the section "Analytical Methods, Instrumentation and Miniaturization".

Deadline for manuscript submissions: closed (30 June 2024) | Viewed by 23667

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Dr. María José Aliaño-González

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1. Department of Analytical Chemistry, University of Cádiz, 11510 Puerto Real, Spain
2. Mediterranean Institute for Agriculture, Environment and Development, University of Algarve, 8005-139 Faro, Portugal
Interests: agrifood resources; forensic chemistry; adulterations; fire analysis; environmental analysis; circular economy; bioactive compounds; chromatography; spectrophotometry; ion mobility spectrometry
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Dr. Bruno Medronho

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1. MED—Mediterranean Institute for Agriculture, Environment and Development, Faculty of Sciences and Technology, University of Algarve, Campus de Gambelas, Ed. 8, 8005-139 Faro, Portugal
2. FSCN, Surface and Colloid Engineering, Mid Sweden University, SE-851 70 Sundsvall, Sweden
Interests: rheology; biopolymers; biomaterials; colloids; lignocellulose; polyphenol dissolution and extraction
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Gas chromatography (GC) is an analytical technique that has been used to separate volatile components from incredibly complex matrices (such as smoke, fuel spills, etc.) and of a very varied nature for their subsequent identification and/or quantification. GC has been coupled to multiple detectors, such as mass spectrometers (MS), which provide significantly high sensitivity (in the ppb range) for the analysis performed and the exact identification of previously separated components. Recently, some researchers have started to use MS as a chemosensor in which each fragment ion (m/z ratio) acts as a sensor and its abundance is equivalent to the signal of this sensor, providing the characteristic total profile of each sample, such as a fingerprint, which allows for the resolution of an analytical problem without the identification of the compounds. This trend has also been observed among other GC-coupled detectors, such as ion mobility spectroscopy or even UV-Vis spectroscopy.

This Special Issue aims to provide a forum for the latest research in the application of gas chromatography and/or mass spectrometry used as chemosensors for analytical purposes. Both review articles and research papers are welcome.

Dr. María José Aliaño-González
Dr. Bruno Medronho
Guest Editors

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Keywords

gas chromatography
mass spectrometry
volatile compounds
total profile
chemosensors
fingerprint
analytical chemistry
complex matrix

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Published Papers (11 papers)

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16 pages, 3525 KiB

Open AccessArticle

Chiral Trapped-Headspace GC-QMS-IMS: Boosting Untargeted Benchtop Volatilomics to the Next Level

by Lukas Bodenbender, Sascha Rohn, Simeon Sauer, Markus Jungen and Philipp Weller

Chemosensors 2024, 12(8), 165; https://doi.org/10.3390/chemosensors12080165 - 17 Aug 2024

Viewed by 1784

Abstract

In the field of quality analysis of food and flavoring products, gas chromatography–quadrupole mass spectrometry–ion mobility spectrometry (GC-QMS-IMS) is a powerful technique for the simultaneous detection of volatile organic compounds (VOCs) by both QMS and IMS. GC is an established technique for the separation of complex VOC-rich food products. While subsequent detection by IMS features soft ionization of fragile compounds (e.g., terpenes) with characteristic drift times, MS provides analytes’ m/z values for database substance identification. A limitation of the prominently used static-headspace-based GC-QMS-IMS systems is the substantially higher sensitivity of IMS in comparison to full-scan QMS. The present study describes a new prototypic trapped-headspace (THS)-GC-QMS-IMS setup using mango purees. This approach ultimately allows the combination of soft ionization with m/z values obtained from database-searchable electron ionization (EI) spectra. The new setup features aligned retention times for IMS and MS and sufficient signal intensities for QMS and IMS. The results demonstrate that THS-GC-QMS-IMS allows for the classification of mango purees from different cultivars and that it could be a promising alternative method for authenticity control of food, flavors, and beverages. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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17 pages, 4876 KiB

Open AccessArticle

Electronic Nose and GC-MS Analysis to Detect Mango Twig Tip Dieback in Mango (Mangifera indica) and Panama Disease (TR4) in Banana (Musa acuminata)

by Wathsala Ratnayake, Stanley E. Bellgard, Hao Wang and Vinuthaa Murthy

Chemosensors 2024, 12(7), 117; https://doi.org/10.3390/chemosensors12070117 - 24 Jun 2024

Cited by 1 | Viewed by 1500

Abstract

Volatile organic compounds (VOCs), as a biological element released from plants, have been correlated with disease status. Although analysis of VOCs using GC-MS is a routine procedure, it has limitations, including being time-consuming, laboratory-based, and requiring specialist training. Electronic nose devices (E-nose) provide a portable and rapid alternative. This is the first pilot study exploring three types of commercially available E-nose to assess how accurately they could detect mango twig tip dieback and Panama disease in bananas. The devices were initially trained and validated on known volatiles, then pure cultures of Pantoea sp., Staphylococcus sp., and Fusarium odoratissimum, and finally, on infected and healthy mango leaves and field-collected, infected banana pseudo-stems. The experiments were repeated three times with six replicates for each host-pathogen pair. The variation between healthy and infected host materials was evaluated using inbuilt data analysis methods, mainly by principal component analysis (PCA) and cross-validation. GC-MS analysis was conducted contemporaneously and identified an 80% similarity between healthy and infected plant material. The portable C 320 was 100% successful in discriminating known volatiles but had a low capability in differentiating healthy and infected plant substrates. The advanced devices (PEN 3/MSEM 160) successfully detected healthy and diseased samples with a high variance. The results suggest that E-noses are more sensitive and accurate in detecting changes of VOCs between healthy and infected plants compared to headspace GC-MS. The study was conducted in controlled laboratory conditions, as E-noses are highly sensitive to surrounding volatiles. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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18 pages, 3224 KiB

Open AccessArticle

HS-SPME-GC/MS Metabolomic Analysis for the Comparative Evaluation between a Plum–Apricot Hybrid and Its Parents

by Anna Lante, Dasha Mihaylova, Ivayla Dincheva and Aneta Popova

Chemosensors 2024, 12(4), 50; https://doi.org/10.3390/chemosensors12040050 - 27 Mar 2024

Cited by 1 | Viewed by 1616

Abstract

The “Stendesto” plumcot is the only successful Bulgarian plum–apricot hybrid having the “Modesto” apricot and the “Stanley” plum as parents. The current study reports on the metabolites and volatile organic compounds (VOCs) discovered in the three fruits. Forty-one metabolites in total, as represented by amino acids, organic acids, sugar acids and alcohols, phenolic acids, fatty acids, mono- and di-saccharides, and sterols, were identified in the samples. Additionally, sixty-five VOCs were profiled using the gas chromatography/mass spectrometry (GC/MS) analysis and HS-SPME technique. Among these VOCs, alcohols, aldehydes, esters, ketones, lactones, terpenoids, and benzene derivatives were the existing chemical classes. Not all metabolites were present in both apricot and plum, but the hybrid had managed to inherit all of the identified metabolites with the exception of γ-aminobutyric acid. This study is a first on the topic of plumcot fruit evaluation referencing its parental lines. Principal component (PCA) and hierarchical cluster (HCA) analyses further aided in revealing the differences and similarities between the “Stendesto” plum–apricot hybrid and its parents. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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26 pages, 2041 KiB

Open AccessArticle

Gas and Liquid Chromatography Mass Spectrometry as a Tool for Elucidating Volatile Organic Compounds (VOCs) and Metabolites in Maternal Milk: A Perspective on Infants’ Health Risk Assessment

by Evangelia N. Tzanetou, Electra Manea-Karga, Eirini Baira, Theodora Boutsikou, Zoi Iliodromiti, Nicoletta Iacovidou, Kyriaki Machera and Konstantinos M. Kasiotis

Chemosensors 2024, 12(3), 30; https://doi.org/10.3390/chemosensors12030030 - 21 Feb 2024

Cited by 1 | Viewed by 2177

Abstract

Maternal milk is pivotal for infants’ nutrition. It also portrays the chemical burden to which the mother has been exposed. One of the chemical families that is prevalent and related to potential toxic effects are volatile organic compounds (VOCs). In the present study, motivated by the scarcity of works dealing with concomitant VOC and metabolite determination in maternal milk, two new gas/liquid chromatography tandem mass spectrometry (GC-MS/MS, LC-MS/MS) methods for the simultaneous measurement of 25 VOCs and 9 of their metabolites, respectively, in maternal milk were developed and applied to 20 maternal milk samples collected from mothers in Greece. In parallel, a headspace solid-phase microextraction (HS-SPME)–GC-MS method was employed for the untargeted screening of chemicals. Low detection rates for benzene, toluene, styrene and p,m-xylenes, and three of their metabolites, namely N-acetyl-S-(benzyl)-L-cysteine (BMA, metabolite of toluene), 3-methylhippuric (3-MHA, metabolite of xylenes) and mandelic acid (MA as DL and R isomers, metabolites of styrene and ethylbenzene), were evidenced in concentrations varying from <lower limit of quantification (LLOQ) to 0.79 ng mL⁻¹. HS-SPME–GC-MS disclosed the presence of common maternal milk constituents such as fatty acids. Nevertheless, bisphenol-A, bisphenol derivatives and phthalates were also detected. The infants’ health risk assessment demonstrated a low risk and negligible carcinogenic risk, yet the detection of these compounds should not be underestimated. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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12 pages, 1153 KiB

Open AccessArticle

Determination of Phenethyl Isothiocyanate, Erucin, Iberverin, and Erucin Nitrile Concentrations in Healthy and Pieris rapae-Infected Broccoli Tissues Using Gas Chromatography-Mass Spectrometry

by Irene-Dimitra Mesimeri, Panagiota-Kyriaki Revelou, Violetta Constantinou-Kokotou and Maroula G. Kokotou

Chemosensors 2024, 12(1), 16; https://doi.org/10.3390/chemosensors12010016 - 22 Jan 2024

Cited by 2 | Viewed by 2079

Abstract

Cruciferous vegetables (Brassicaceae family) are a rich source of phytochemicals, in particular glucosinolates (GLS) and their hydrolysis products, isothiocyanates and nitriles. These phytochemicals may act as chemosensors, attracting insects, such as Pieris rapae, and stimulating oviposition. There is a lack of information on the concentrations of isothiocyanates and nitriles when an insect affects a Brassicaceae plant. In the current study, some GLS hydrolysis products were determined in healthy and Pieris rapae-infected organic cultivated broccoli plants, as well as the infesting insects’ larvae, using gas chromatography-mass spectrometry (GC-MS). This study investigated the following phytochemicals: phenethyl isothiocyanate (PEITC), erucin (ER), 3-(methylthio)propyl isothiocyanate (3MIC), and 1-cyano-4-(methylthio)butane (5MITN). All these components were quantified in the aerial and underground parts of the plants and were found in high concentrations in the roots. Among the phytochemicals studied, 5MITN presented the highest concentration in all the broccoli samples but was especially high in the stalks of the infected plants. Moreover, the analysis of a sample of Pieris rapae larvae, fed from the hosted broccoli, revealed the presence of PEITC and ER. These findings indicate that the infestation of broccoli with Pieris rapae may affect the distribution of PEITC, ER, 3MIC, and 5MITN throughout the plant. An extension of our study to conventional cultivated broccoli showed that the roots are indeed rich in GLS hydrolysis products. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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18 pages, 1436 KiB

Open AccessArticle

Evaluation of the Essential Oil Composition of Five Thymus Species Native to Greece

by Eleni Kakouri, Dimitra Daferera, Anastasia Andriopoulou, Panayiotis Trigas and Petros A. Tarantilis

Chemosensors 2024, 12(1), 7; https://doi.org/10.3390/chemosensors12010007 - 31 Dec 2023

Viewed by 3001

Abstract

The genus Thymus encompasses a wide array of taxa, many of which remain underexplored in terms of their phytochemical profile. In this study, we investigated the phytochemical composition of volatile compounds of five Thymus species native to Greece using gas chromatography combined with mass spectrometry. Two samples of T. parnassicus collected from Mts Parnitha and Parnassos were studied. The predominant compounds in the Parnitha sample were α-cadinol (13.53%), E-caryophyllene (11.83%) and selin-11-en-4α-ol (7.29%). The sample from Mt. Parnassos exhibited a high concentration of E-caryophyllene (35.20%) followed by β-bisabolene (10.41%). Additionally, two species, namely T. leucotrichus subsp. leucotrichus and T. atticus, were collected on Mt. Chelmos (Peloponnese). The essential oil of T. leucotrichus was rich in elemol (35.56%), α-eudesmol (11.15%) and β-eudesmol (6.11%). Thymus atticus exhibited a high concentration in linalool (63.04%) and p-cymene (25.63%). In addition, two samples of T. holosericeus collected from Kefalonia Ιsland were both rich in geraniol (89.9% and 87.7%, respectively). We also examined the volatile profile of T. laconicus, a local endemic species of SE Peloponnese (Lakonia area), which remains unexplored. Carvacrol (32.7%) and p-cymene (29.7%) were identified as the dominant compounds. Our study contributes valuable insights into the chemical profile of Thymus spp. and sheds further light on the well-known chemical polymorphism within this genus. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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23 pages, 2653 KiB

Open AccessArticle

Modifying Headspace Sampling Environment Improves Detection of Boar Taint Compounds in Pork Fat Samples

by Clément Burgeon, Alice Markey, Yves Brostaux and Marie-Laure Fauconnier

Chemosensors 2023, 11(11), 551; https://doi.org/10.3390/chemosensors11110551 - 28 Oct 2023

Viewed by 1758

Abstract

The extraction of boar taint compounds from pork fat samples was performed under various temperature (150, 300 and 450 °C) and atmosphere (air, nitrogen and reduced pressure) conditions. This aimed at understanding which conditions allow the greatest extractions of indole, skatole and androstenone (present in backfat in low concentrations) while limiting the presence of other VOCs in the headspace of heated fat (interfering with correct VOC-based detection of boar taint compounds). Indole and skatole were extracted in the greatest concentrations when heating backfat at 450 °C under reduced pressure, while androstenone was highest when heating at 300 °C under reduced pressure. Oxidation products were most abundant under air conditions, nitrogenated products appeared in the presence of a nitrogen-enriched atmosphere, and lastly, molecules intrinsic to boar fat saw their headspace concentration increase with reduced pressure. The combination of 450 °C and reduced pressure atmosphere was suggested for the heating of backfat prior to detection with analytical methods and to complement the current sensory analysis. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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22 pages, 1778 KiB

Open AccessArticle

Solid-Phase Extraction Followed by Gas Chromatography–Mass Spectrometry for Revealing the Effects of the Application of Bentonite, Tannins, and Their Combination during Fermentation in the Production of White Wine

by Igor Lukić, Ivana Horvat, Sanja Radeka and Urska Vrhovsek

Chemosensors 2023, 11(10), 545; https://doi.org/10.3390/chemosensors11100545 - 21 Oct 2023

Cited by 2 | Viewed by 2365

Abstract

To investigate the effects of the application of bentonite, tannins, and their combination in alcoholic fermentation, Malvazija istarska (Vitis vinifera L.) white grape must was treated with 95 g/L of bentonite, 25 g/L of a hydrolysable tannin preparation, while the third treatment received the aforementioned doses of both agents. Control grape must was fermented without bentonite and exogenous tannins. All of the produced wines were additionally fined after fermentation with doses of bentonite needed to achieve complete protein stability. Wines were analyzed both after fermentation and after additional bentonite fining. Standard physicochemical parameters were determined by the OIV methods, and phenols were analyzed by high-performance liquid chromatography with diode-array detection (HPLC-DAD), while the concentrations of free and bound volatile aroma compounds were obtained after solid-phase extraction (SPE) followed by gas chromatography–mass spectrometry (GC-MS). Bentonite and tannins in fermentation generally reduced the total dose of bentonite needed for complete stabilization. Treatments with bentonite slightly decreased the concentration of total dry extract, while tannins preserved total acidity. The negative effect of bentonite on flavonoids was more severe. Tannins in fermentation preserved more hydroxycinnamoyltartaric acids with respect to control wine, and this effect was additionally enhanced by bentonite. Volatile and bound aroma composition was affected by all the treatments, while the addition of tannins resulted in higher concentrations of several important odoriferous esters, such as ethyl hexanoate, ethyl decanoate, and hexyl acetate. Additional fining with bentonite to complete protein stabilization annulled some of the positive effects observed after fermentation. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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15 pages, 3869 KiB

Open AccessArticle

Method Comparison for the Identification and Characterization of Odorants from Scots Pine (Pinus sylvestris L.) and Oriented Strand Boards (OSB) Made Thereof by GC-MS and GC-FID/O Using Different Headspace Techniques

by Valentin Schierer, Cornelia Rieder-Gradinger and Erwin Rosenberg

Chemosensors 2023, 11(10), 543; https://doi.org/10.3390/chemosensors11100543 - 19 Oct 2023

Viewed by 2191

Abstract

Volatile organic compounds (VOCs) from wood and wood composites are important contributors to odor profiles of indoor environments and can significantly influence human health and well-being. GC-MS/FID and gas chromatography (GC) with olfactometric detection (GC-O) are employed for the identification and characterization of odorants. Four different sample preparation methods are evaluated on wood strands and isocyanate adhesive–based oriented strand boards (OSBs) made from Pinus sylvestris L.: among these, dynamic headspace extraction thermal desorption ((dynamic) HS-TD), head space solid phase microextraction (HS-SPME), head space solid phase microextraction Arrow (HS-SPME Arrow), and liquid injection of a CH₂Cl₂ solvent extract. The olfactometric investigation revealed over 30 odor-active substances of cyclic and acyclic monoterpene, monoterpenoid ketone, monoterpenoid aldehyde, monoterpenoid alcohol, monoterpenoid ester, aliphatic aldehyde, alcohol, and acid and phenolic chemistry. Compared to liquid injection, (dynamic) HS-TD was found to result in a similar number of odorants (20 vs. 24), whereas HS SPME Arrow shows good performance with minimal instrumental effort, notably for monoterpene and aldehyde compounds. Native wood vs. OSB showed high concentrations of saturated and unsaturated aldehydes for the wood board sample. These findings demonstrate the capability of headspace methods for odorant detection and their suitability for standardization towards a database for wood and wood composites. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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13 pages, 3838 KiB

Open AccessArticle

Solid-Phase Microextraction (SPME) and Gas Chromatographic/Mass Spectrometry in Chronic Obstructive Pulmonary Disease (COPD): A Chemometric Approach

by Loukia Lypirou, Christos Chronis, Konstantinos Exarchos, Konstantinos Kostikas and Vasilios Sakkas

Chemosensors 2023, 11(10), 542; https://doi.org/10.3390/chemosensors11100542 - 18 Oct 2023

Viewed by 2039

Abstract

Chronic Obstructive Pulmonary Disease (COPD) is a chronic respiratory condition that often goes undiagnosed despite the availability of spirometry for diagnosis, and its exact prevalence remains uncertain. Exhaled breath has been proposed as a source of relevant health information, particularly Volatile Organic Compounds (VOCs), which can be easily obtained and applied in clinical practice. In this study, exhaled breath samples were collected from patients diagnosed with COPD of varying severity during their stable condition using specialized RTubeVOC tubes. Volatile compounds from the air samples were extracted using a 50/30 µm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber and the analysis was performed using gas chromatography/mass spectrometry (GC/MS) technique. The patients were divided into two groups based on their history of exacerbations, and the aim was to identify VOCs associated with the risk of future COPD exacerbation, thus allowing for more personalized and objective COPD treatment. Blood eosinophil content was also taken into consideration. A panel of distinguishing mass-spectral features was identified between the two patient groups. The discriminating exhaled molecules were heptane 2,2,4,6,6-pentamethyl, gamma-terpinene, 2-ethylhexanol, and undecane demonstrating the potential of analyzing VOCs in exhaled breath for the detection and management of COPD, offering a promising avenue to improve COPD management and treatment approaches. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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8 pages, 769 KiB

Open AccessBrief Report

Validation of a Headspace Gas Chromatography with Flame Ionization Detection Method to Quantify Blood Alcohol Concentration (BAC) for Forensic Practice

by Alice Cerioni, Gianmario Mietti, Marta Cippitelli, Giulia Ricchezze, Erika Buratti, Rino Froldi, Mariano Cingolani and Roberto Scendoni

Chemosensors 2024, 12(7), 133; https://doi.org/10.3390/chemosensors12070133 - 9 Jul 2024

Cited by 2 | Viewed by 2019

Abstract

Alcohol consumption is a major social and forensic issue. It is often the cause of road accidents, industrial accidents, suicides and other crimes. On account of this, it is of fundamental importance in forensic toxicology to correctly quantify blood alcohol concentration (BAC). In this work, a straightforward method for the quantification of ethanol from blood samples by means of headspace gas chromatography with flame ionization detection is presented and validated. For method validation linearity, limit of detection (LOD), lower limit of quantification (LLOQ), accuracy, precision (% CV) and interference studies were carried out. All the validation conditions were satisfied according to the acceptance criteria. Proof of applicability was performed on 50 real blood samples, showing that the method was effective. Full article

(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges (Second Edition))

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