GC, MS and GC-MS Analytical Methods: Opportunities and Challenges

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 (31 August 2023) | Viewed by 33629

Special Issue Editors


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Guest Editor
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
Special Issues, Collections and Topics in MDPI journals

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Guest Editor
Department of Chemistry and Physics, University of Almeria, Almeria, Spain
Interests: trace analysis; environmental pollution; food safety; bioactive compounds; food quality; sample preparation; chromatography; high resolution mass spectrometry

E-Mail Website
Guest Editor
Department of Chemistry and Physics, Universidad de Almería, Almeria, Spain
Interests: food safety; pesticides; analytical method development; chromatography; mass spectrometry; high-performance liquid chromatography
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

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

The Special Issue "GC, MS and GC-MS Analytical Methods: Opportunities and Challenges" aims to provide a forum for the latest research on 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. Irene Domínguez Pérez
Prof. Dr. Roberto Romero-González
Guest Editors

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Keywords

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

Published Papers (18 papers)

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18 pages, 1683 KiB  
Article
Assessment of Volatile Characteristics of Okinawan Pineapple Breeding Lines by Gas-Chromatography–Mass-Spectrometry-Based Electronic Nose Profiling and Odor Activity Value Calculation
by Yonathan Asikin, Mutsumi Kawahara, Sora Kochi, Ryota Maekawa, Yuta Omine, Makoto Takeuchi, Kensaku Takara and Koji Wada
Chemosensors 2023, 11(10), 512; https://doi.org/10.3390/chemosensors11100512 - 28 Sep 2023
Viewed by 1168
Abstract
The recent increase in demand for Okinawan pineapples has necessitated the development of new varieties with attractive aromas. This study aimed to evaluate the volatile characteristics of five Okinawan pineapple breeding lines, i.e., ‘No. 22’, ‘No. 25’, ‘No. 26’, ‘No. 27’, and ‘No. [...] Read more.
The recent increase in demand for Okinawan pineapples has necessitated the development of new varieties with attractive aromas. This study aimed to evaluate the volatile characteristics of five Okinawan pineapple breeding lines, i.e., ‘No. 22’, ‘No. 25’, ‘No. 26’, ‘No. 27’, and ‘No. 28’. The total volatiles in the cryopulverized fruit flesh were examined using headspace gas-chromatography–mass-spectrometry-based electronic nose analysis. The total ion masses of the volatiles were visualized using principal component analysis, and three replicates of each line with comparable volatile characteristics were selected. Furthermore, the composition of the volatile components in these replicates was assessed, and the odor activity values (OAVs) were calculated. The breeding lines varied in the quantity and composition of their volatile compounds, which were predominantly esters, ketones, terpenes, and alcohols. The ‘No. 22’ fruit contained a greater content of volatiles than the other lines. Moreover, 14 volatiles with OAV > 1 were accounted as aroma-active compounds, and their variations were distinguished as follows: the highest OAV (786.96) was recorded for methyl 2-methylbutanoate of the ‘No. 26’ line; 2,5-dimethyl-4-methoxy-3(2H)-furanone was superior in the ‘No. 26’ and ‘No. 27’ lines; and δ-decalactone was only present in the ‘No. 22’ and ‘No. 27’ fruits, suggesting different potent practical uses for these new breeding lines. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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17 pages, 3025 KiB  
Article
Simultaneous Detection and Quantification of Aflatoxin M1, Eight Microcystin Congeners and Nodularin in Dairy Milk by LC-MS/MS
by Camille Van Camp, Wannes Hugo R. Van Hassel, Mohamed F. Abdallah and Julien Masquelier
Chemosensors 2023, 11(10), 511; https://doi.org/10.3390/chemosensors11100511 - 25 Sep 2023
Viewed by 1160
Abstract
Dairy milk holds a prominent position as a widely consumed food, particularly among infants and children. However, it is crucial to address the presence of multiple natural toxic compounds that may co-occur in dairy milk to ensure its safety prior to consumption. Aflatoxin [...] Read more.
Dairy milk holds a prominent position as a widely consumed food, particularly among infants and children. However, it is crucial to address the presence of multiple natural toxic compounds that may co-occur in dairy milk to ensure its safety prior to consumption. Aflatoxin M1 (AFM1), an emerging mycotoxin of interest, is a potential contaminant in the milk of animals who ingest aflatoxin B1 (AFB1). The toxin is regulated in the European Union under Commission Regulation No 1881/2006. Unfortunately, there is a notable lack of data concerning the transfer of various emerging microbial contaminants into dairy milk and, therefore, their natural occurrences. In this study, a simple and sensitive LC-MS/MS method was developed and validated for the quantification of multiple cyanotoxins (microcystin congeners and nodularin) and AFM1 by the main analytical guidelines. Toxins are extracted with methanol 80%, followed by an SPE clean-up step before LC-MS/MS analysis. The LOQ was fixed at 1 µg/L for the nine cyanotoxins and 0.05 µg/L for AFM1. Recoveries were measured between 82.67% and 102%. To the best of our knowledge, there are no other LC-MS/MS methods available for the simultaneous quantification of cyanotoxins and mycotoxins in milk. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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14 pages, 1665 KiB  
Article
Development and Validation of a Solvent-Free Headspace GC-MS Method for the Screening of Benzyl Chloride in Pharmaceutical Products
by Eunchae Song, Chanhong Min, Eunjae Kim, Sang Beom Han, Yong-Moon Lee, Kwang-Hyeon Liu, Jongki Hong and Han Bin Oh
Chemosensors 2023, 11(9), 487; https://doi.org/10.3390/chemosensors11090487 - 03 Sep 2023
Viewed by 1477
Abstract
This study presents a solvent-free headspace gas chromatography–mass spectrometry (SF-HS-GC/MS) method for robustly screening benzyl chloride, a mutagenic carcinogen, impurities in active pharmaceutical ingredients (APIs) and drug products. The SF-HS-GC/MS method simplifies analysis by eliminating solvent use, reducing matrix interference. Optimized headspace parameters [...] Read more.
This study presents a solvent-free headspace gas chromatography–mass spectrometry (SF-HS-GC/MS) method for robustly screening benzyl chloride, a mutagenic carcinogen, impurities in active pharmaceutical ingredients (APIs) and drug products. The SF-HS-GC/MS method simplifies analysis by eliminating solvent use, reducing matrix interference. Optimized headspace parameters include incubation temperature, time, and sample amount. Validation, aligned with Q2(R1) ICH guidelines and ICH M7 recommendations, covers selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, system suitability, and robustness. Employing a DB-5MS column (30 m × 0.25 mm, 0.25 µm) with solvent-free split injection, the method’s calibration curve (0.05–5 μg/g) exhibits a strong correlation (>0.9998). The LOQ was 0.1 μg/g, with precision (%CV) consistently <5% and accuracy within 95–105%. Furthermore, an investigation confirmed the absence of artefactual benzyl chloride formation in drug products under headspace conditions. The developed SF-HS-GC/MS method successfully screened benzyl chloride in cinnarizine drug substances and products. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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11 pages, 1355 KiB  
Article
GC/MS Profile and Antifungal Activity of Zanthoxylum caribaeum Lam Essential Oil against Moniliophthora roreri Cif and Par, a Pathogen That Infects Theobroma cacao L Crops in the Tropics
by Marcial Fuentes-Estrada, Andrea Jiménez-González, Diannefair Duarte, Rogerio Saavedra-Barrera, Carlos Areche, Elena Stashenko, Nayive Pino Benítez, Daniela Bárcenas-Pérez, José Cheel and Olimpo García-Beltrán
Chemosensors 2023, 11(8), 447; https://doi.org/10.3390/chemosensors11080447 - 10 Aug 2023
Viewed by 1012
Abstract
The species Zanthoxylum caribaeum belongs to the Rutaceae family, from which several chemical nuclei are known, including alkaloids and coumarins. In addition, its essential oil has been characterized, showing differences in composition and various antimicrobial activities. In the present study, the essential oil [...] Read more.
The species Zanthoxylum caribaeum belongs to the Rutaceae family, from which several chemical nuclei are known, including alkaloids and coumarins. In addition, its essential oil has been characterized, showing differences in composition and various antimicrobial activities. In the present study, the essential oil of Z. caribaeum collected in the department of Tolima, central Colombia, was characterized by gas chromatography with mass selective detector (GC-MS). The essential oil showed a composition of about 43 compounds (including major and minor), whose main components, according to their abundance, are the following: germacrene D (228.0 ± 1.6 mg/g EO), (E)-β-farnesene (128.0 ± 1.5 mg/g EO), β-elemene (116.0 ± 1.6 mg/g EO) and (E)-nerolidol (74.0 ± 2.2 mg/g EO). This oil was tested against microorganisms that affect cocoa production in Colombia and in tropical countries where the production of this commodity is very important for the economy. The antifungal tests were performed on the fungal species Moniliophthora roreri and showed promising and significant activity, inhibiting growth by more than 95% at concentrations of 50 µL/mL and 100 µL/mL. This remarkable antifungal activity could be due to the presence of major and minor compounds that synergistically enhance the activity. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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21 pages, 1825 KiB  
Article
Volatile Compound Profile Analysis of Seasonal Flower, Fruit, Leaf, and Stem of Zanthoxylum armatum DC. from Manipur Using HS-SPME-GC-MS
by Moirangthem Lakshmipriyari Devi, Nameirakpam Bunindro Singh, Kongbrailatpam Chandradev Sharma, Yallappa Rajashekar, Amrita Mishra and Sudripta Das
Chemosensors 2023, 11(5), 273; https://doi.org/10.3390/chemosensors11050273 - 02 May 2023
Cited by 1 | Viewed by 1405
Abstract
In the present study, GC-MS analyses were performed with powder samples of flower, fruit, leaf, and stem of Zanthoxylum armatum DC. collected from Thambalkhong, Imphal-East district of Manipur, a north-eastern region of India, based on the season and growth stage of the plant [...] Read more.
In the present study, GC-MS analyses were performed with powder samples of flower, fruit, leaf, and stem of Zanthoxylum armatum DC. collected from Thambalkhong, Imphal-East district of Manipur, a north-eastern region of India, based on the season and growth stage of the plant using the extraction method headspace solid-phase microextraction (HS-SPME) to study the total profile of volatile compounds. Variations were discovered in the volatile compound profiles. HS-SPME-GC-MS analyses of the plant parts detected and identified 16 to 36 compounds and found a total area percentage composition of 96.81 to 98.63%. The analysis showed that nine common compounds were detected in the studied plant parts and seasons, namely, α-thujene, α-pinene, sabinene, β-pinene, terpinolene, o-cymene, sylvestrene, eucalyptol, and caryophyllene. The monoterpenoid eucalyptol (1,8-cineole) was revealed to be the principal component with an area percentage composition of 31.02% in spring leaf to 73.16% in monsoon stem. The extraction method used in this investigation was very fast and feasible for the analysis, and the findings of the present study will help understand the mechanism behind the changes in the plant’s volatile organic compound profile and future research work for selecting aroma-rich accessions for targeted improvement of this plant. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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14 pages, 1933 KiB  
Article
Validation of a HS–GC–FID Method for the Quantification of Sevoflurane in the Blood, Urine, Brain and Lungs for Forensic Purposes
by Guido Pelletti, Rossella Barone, Susan Mohamed, Francesca Rossi, Marco Garagnani, Arianna Giorgetti, Paolo Fais and Susi Pelotti
Chemosensors 2023, 11(2), 133; https://doi.org/10.3390/chemosensors11020133 - 13 Feb 2023
Cited by 1 | Viewed by 1861
Abstract
Background: Sevoflurane is a polyfluorinated compound extensively used as an inhalation anesthetic in patients undergoing surgery. If administered outside the operating room, sevoflurane is dangerous and potentially lethal, and toxicologists may be asked to investigate its presence in biological matrices for forensic purposes. [...] Read more.
Background: Sevoflurane is a polyfluorinated compound extensively used as an inhalation anesthetic in patients undergoing surgery. If administered outside the operating room, sevoflurane is dangerous and potentially lethal, and toxicologists may be asked to investigate its presence in biological matrices for forensic purposes. The aim of the present study is to develop and validate a method for the detection and the quantification of sevoflurane in biological fluids and organs through gas chromatography coupled to flame ionization detection (GC–FID). Methods: The method was optimized based on the maximization of the signal-to-noise ratio. The GC–FID instrument was equipped with a Zebron capillary column ZB-624 (30 m, 0.32 mm ID, 1.80 µm film thickness). Results: The method was validated over a concentration range of 1.0–304.0 µg/mL (blood and urine) and µg/g (brain, lungs). The lower limit of quantitation was 1.0 µg/mL or µg/g. Both the intra- and interassay imprecision and inaccuracy were ≤15% at all quality control concentrations in all the matrices. The method was successfully applied to measure the sevoflurane concentrations for 20 negative controls and for a real forensic case. Conclusions: The present method is suitable for the identification and quantification of sevoflurane in fluids and organs and can be a reliable tool in forensic casework. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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16 pages, 2313 KiB  
Article
Evaluation of the Transfer and Occurrence of Opium Alkaloids in Poppy Seed Teas Using Preconcentrations with µSPEed® Followed by GC-MS Analysis
by Gema Casado-Hidalgo, Rosa Perestelo, Sonia Morante-Zarcero, José S. Câmara and Isabel Sierra
Chemosensors 2023, 11(2), 94; https://doi.org/10.3390/chemosensors11020094 - 27 Jan 2023
Cited by 4 | Viewed by 1792
Abstract
Intoxication due to the consumption of poppy seed teas has been reported due to their contamination with opium alkaloids (OAs). In this work, an efficient methodology based on microsolid-phase extraction (µSPEed®) followed by gas chromatography–mass spectrometry (GC-MS) has been optimized to [...] Read more.
Intoxication due to the consumption of poppy seed teas has been reported due to their contamination with opium alkaloids (OAs). In this work, an efficient methodology based on microsolid-phase extraction (µSPEed®) followed by gas chromatography–mass spectrometry (GC-MS) has been optimized to quantify five OAs in poppy seed teas. Nine cartridges (C4, C8, C18, silica, APS, PFAs, PS/DVB-RP, PS/DVB-SCX and PS/DVB-SAX), pH levels, cycles and elution solvents were evaluated. The method was validated and applied to study the transfer of OAs by evaluating water temperatures, infusion times and seed amounts. The highest transfer rates (71% for morphine, 96% for thebaine, and 100% for codeine, noscapine and papaverine) were achieved at 90°C, 5 min, with 4 g. These conditions were used to quantify the OAs in four teas prepared from different seeds. A high amount of morphine (1563 µg/L) was found in one tea, indicating that the seeds had a concentration twice the maximum limit, highlighting the need to warn the population of this dangerous practice. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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13 pages, 2061 KiB  
Article
E-Nose Quality Evaluation of Extra Virgin Olive Oil Stored in Different Containers
by Elísabet Martín-Tornero, Juan Diego Barea-Ramos, Jesús Lozano, Isabel Durán-Merás and Daniel Martín-Vertedor
Chemosensors 2023, 11(2), 85; https://doi.org/10.3390/chemosensors11020085 - 21 Jan 2023
Cited by 7 | Viewed by 1858
Abstract
The degradation process of virgin olive oil (VOO) is related to storage time and the type of storage container used. The aim of this work is to explore the evolution of the VOO quality stored in different container types over a defined storage [...] Read more.
The degradation process of virgin olive oil (VOO) is related to storage time and the type of storage container used. The aim of this work is to explore the evolution of the VOO quality stored in different container types over a defined storage period in order to predict the organoleptic characteristics using a non-destructive technique such as the electronic-nose (E-nose). The “Picual” variety VOO was stored in different containers over a period of 21 months and monitored using sensory analysis, volatile compounds, and an E-nose. The panelists showed that oil stored in dark glass bottles and in green polyethylene bottles began to show defects after 12 and 15 weeks, respectively. However, oil stored in tin containers retained its quality throughout the 21 months studied. A total of 31 volatile compounds were identified, and the evolution of the volatile profile in the different containers during the storage period was studied. The E-nose data were able to classify oil quality by container using principal component analysis (PCA). Furthermore, the E-nose data combined with partial least squares (PLS) regression enabled the building of a predictive model to quantify sensory defect values (RCV2 = 0.92; RCV2 = 0.86), evidencing that this technique would be an appropriate screening tool to support a sensory panel. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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12 pages, 1822 KiB  
Article
HS-SPME-GC/MS Method for the Simultaneous Determination of Trihalomethanes, Geosmin, and 2-Methylisoborneol in Water Samples
by Diego Pardina, Asier Santamaria, María Luz Alonso, Luis Bartolomé, Rosa M. Alonso, Jon Ander Maña, Elisabeth Bilbao, Jose Ignacio Lombraña, Mikel Bartolome and Luis M. Hernando
Chemosensors 2023, 11(2), 84; https://doi.org/10.3390/chemosensors11020084 - 21 Jan 2023
Cited by 4 | Viewed by 2562
Abstract
Drinking water treatment plants (DWTP) use chlorination as an oxidation stage in the first step of the processes used to eliminate the natural organic matter (NOM) responsible for the formation of 2-methylisoborneol (2-MIB) and Geosmin (GM), which produce odor and taste to the [...] Read more.
Drinking water treatment plants (DWTP) use chlorination as an oxidation stage in the first step of the processes used to eliminate the natural organic matter (NOM) responsible for the formation of 2-methylisoborneol (2-MIB) and Geosmin (GM), which produce odor and taste to the water. However, chlorination processes give rise to disinfectant toxic subproducts, such as trihalomethanes (THMs). In this work, a headspace solid-phase microextraction coupled with a gas chromatography/mass spectrometric method has been developed for the quality control of drinking water. 2-MIB, GM, and THMs at different stages of the drinking water treatment process were monitored. The method was validated following the Environmental Protection Agency guidelines. Neither carryover nor the matrix effect was observed. The performance of the method was satisfactory in terms of selectivity, repeatability, and accuracy and exhibited a linear concentration range of 0.8–50 µg/L for trichloromethane (TCM), 0.05–20 µg/L for bromodichloromethane, 0.01–20 µg/L for dibromochloromethane and tribromomethane, and 0.005–0.05 µg/L for GM and 2-MIB. The THMs concentration obtained for all the water samples was below the thresholds established by international organizations and, for 2-MIB and GM, were lower for their limit of quantification. The method was also applied to the adsorption kinetic study of TCM on granulated activated carbon, which is the main barrier to reducing the NOM in DWTP. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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14 pages, 2445 KiB  
Article
Effect of Cultivar and Geographical Origin on the Volatile Composition of Greek Monovarietal Extra Virgin Olive Oils
by Theano Mikrou, Maria Litsa, Artemis Papantoni, Maria Kapsokefalou, Chrysavgi Gardeli and Athanasios Mallouchos
Chemosensors 2023, 11(2), 80; https://doi.org/10.3390/chemosensors11020080 - 21 Jan 2023
Cited by 5 | Viewed by 1323
Abstract
Extra virgin olive oil (EVOO) is highly appreciated by consumers for its unique sensory characteristics that are directly related to its volatile composition. The objective of this study was to investigate the effect of cultivar and geographical origin on the volatile composition of [...] Read more.
Extra virgin olive oil (EVOO) is highly appreciated by consumers for its unique sensory characteristics that are directly related to its volatile composition. The objective of this study was to investigate the effect of cultivar and geographical origin on the volatile composition of Greek monovarietal EVOOs. Samples of three local cultivars (Koroneiki, Kolovi and Adramytini) originating from three areas of Greece (Crete, Lesvos and the Peloponnese), spanning two consecutive harvesting periods, were selected. Their volatile components were determined using headspace solid-phase microextraction combined with gas chromatography–mass spectrometry. More than 70 volatile compounds were identified. Alcohols were the dominant class (43–50%), followed by ketones (12–24%), esters (12–18%) and aldehydes (4–12%). The most prominent volatile compounds were (Z)-3-hexen-1-ol (6–11%), 1-penten-3-ol (7–11%), (E)-3-hexenyl acetate (0.5–11%) and 3-pentanone (8–16%). Significant differences were observed and highlighted. Clear separations between samples from different cultivars and geographic provenances were achieved using multivariate analysis and the most discriminating volatiles were identified. Additionally, using multivariate receiver operating characteristic (ROC) curve analysis, a combination of five chemical markers was found superior (area under the curve, AUC: 1.00; predictive accuracy: 100%) for the correct classification of Koroneiki EVOOs according to geographical origin. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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12 pages, 3879 KiB  
Communication
Gas Chromatography Fingerprint of Martian Amino Acids before Analysis of Return Samples
by Rihab Fkiri, Ramzi Timoumi, Guillaume Rioland, Pauline Poinot, Fabien Baron, Brian Gregoire and Claude Geffroy-Rodier
Chemosensors 2023, 11(2), 76; https://doi.org/10.3390/chemosensors11020076 - 18 Jan 2023
Viewed by 1364
Abstract
Within the perspective of the current and future space missions, the detection and separation of building blocks such as amino acids are important subjects which are becoming fundamental in the search for the origin of life and traces of life in the solar [...] Read more.
Within the perspective of the current and future space missions, the detection and separation of building blocks such as amino acids are important subjects which are becoming fundamental in the search for the origin of life and traces of life in the solar system. In this work, we have developed and optimized a strategy adapted to space experimentation to detect the presence of amino acid-like compounds using gas chromatography coupled to mass spectrometry (GC-MS). Selected derivatization methods meet the instrument design constraints imposed on in situ extraterrestrial experiments. Coupled to a fast selective extraction, GC analysis would be highly efficient for the detection of organic materials. In the future, the corresponding GC-MS TIC could facilitate simple and fast selection of sediments/dust samples onboard GC-MS-equipped rovers for sample return-to-Earth missions. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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17 pages, 1110 KiB  
Article
Target and Suspect Analysis with High-Resolution Mass Spectrometry for the Exhaustive Monitoring of PCBs and Pesticides in Posidonia oceanica Meadows and Sediments
by Marina Astudillo-Pascual, Pedro A. Aguilera, Antonia Garrido Frenich and Irene Domínguez
Chemosensors 2022, 10(12), 531; https://doi.org/10.3390/chemosensors10120531 - 12 Dec 2022
Cited by 1 | Viewed by 1415
Abstract
This study enables the simultaneous monitoring of persistent organics pollutants (POPs) in the relevant marine seagrass Posidonia oceanica (L.) Delile (P. oceanica), without causing damage and preserving their ecological integrity and their key ecosystem services, and in marine sediments. Two classes [...] Read more.
This study enables the simultaneous monitoring of persistent organics pollutants (POPs) in the relevant marine seagrass Posidonia oceanica (L.) Delile (P. oceanica), without causing damage and preserving their ecological integrity and their key ecosystem services, and in marine sediments. Two classes of POPs that suppose a current threat to the environmental health status are investigated: polychlorinated biphenyls (PCBs) and pesticides. Comparisons between tissues and sediment compartmentation are studied for the first time. For these purposes, the sediments, P. oceanica leaves and, as a novelty, rhizomes, were studied. Samples were analyzed by gas chromatography coupled with high-resolution mass spectrometry (GC-Q-Orbitrap MS) for a comprehensive study. Eco-friendly methods were developed and validated for the determination of 38 POPs, 25 PCBs and 13 priority pesticides. The results showed that, when detected, regulated contaminants were localized mainly in the long-lived rhizomes, and 7 PCBs (the most abundant being PCB 44) and 4 priority pesticides (trifluralin, chlorpyrifos, isodrin and o,p’-DDT) were seen. Additionally, a retrospective analysis (suspect screening) was conducted, exhibiting up to 13 current-use pesticide residues in leaves and rhizomes alike. The results suggest that P. oceanica might be acting as a sink to contaminants in coastal areas and that rhizomes, due to their longer lifespan, reflect past and legacy contamination. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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13 pages, 1123 KiB  
Article
Screening of Chemical Composition, Antimicrobial and Antioxidant Activities of Essential Oil and Volatile Fraction from Olive Mill Wastewater
by Chahinez Ait Si Said, Nacera Riad, Mohamed Reda Zahi, Smain Sabour, Salah Akkal, Wissam Zam, Ouassila Touafek and Mohamed El Hattab
Chemosensors 2022, 10(11), 491; https://doi.org/10.3390/chemosensors10110491 - 19 Nov 2022
Cited by 5 | Viewed by 1507
Abstract
Oil mill wastewater is the main by-product of the olive oil industry resulting mainly from the treatment and pressing of olives in mills. It is a rich source of nutrients and phytochemicals with a wide spectrum of biological properties. The present study focuses [...] Read more.
Oil mill wastewater is the main by-product of the olive oil industry resulting mainly from the treatment and pressing of olives in mills. It is a rich source of nutrients and phytochemicals with a wide spectrum of biological properties. The present study focuses on the chemical analysis and evaluation of the antimicrobial and antioxidant activity of the essential oil (EO) and the volatile fraction (VF) obtained, respectively, by hydrodistillation. Chemical analysis by gas chromatography coupled to mass spectrometry (GC/MS) and a flame ionisation detector (GC/FID) revealed the predominance of phenolic compounds (25.71%, 60.36%) and fatty acids (62.37%, 38.25%) for the VF and EO, respectively. It was also shown that the main compounds were oleic acid (24.9%) for the VF and 4-ethylphenol (28.5%) for the EO. The results of the antimicrobial activity in terms of MIC values against twelve microorganisms showed that, overall, the VF was more active than the EO. The antioxidant activity of the VF and EO was evaluated using the DPPH assay and expressed as half-maximal inhibitory concentration (IC50), where the EO (218 μg/mL) showed better antioxidant activity than the VF (244 μg/mL). The results also revealed that the antimicrobial activity and antioxidant activity values for both oils were significantly lower than the standards used. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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12 pages, 1573 KiB  
Article
Biomonitoring and Assessment of Dumpsites Soil Using Phospholipid Fatty Acid Analysis (PLFA) Method—Evaluation of Possibilities and Limitations
by Judit Halász, Zsolt Kotroczó, Péter Szabó and Tamás Kocsis
Chemosensors 2022, 10(10), 409; https://doi.org/10.3390/chemosensors10100409 - 10 Oct 2022
Cited by 1 | Viewed by 1630
Abstract
Dumped waste is not only a problem from an aesthetic point of view, but also has an environmental polluting effect, or can even pose a direct danger if the waste is dumped in illegal landfills in an uncontrolled manner with unknown composition. In [...] Read more.
Dumped waste is not only a problem from an aesthetic point of view, but also has an environmental polluting effect, or can even pose a direct danger if the waste is dumped in illegal landfills in an uncontrolled manner with unknown composition. In the case of soil pollution, the assessment of the changing microbial state can be used as an indicator of initial changes, since waste as a pollutant impacts the diversity of the landfill’s microbial community. The degree of change depends on the qualitative and quantitative composition of the pollutants, which can be measured through the microbial phospholipid fatty acid (PLFA) pattern. The aim was a comprehensive assessment of the soil microbiological and toxicological hazards of various illegal landfill. Cluster-analysis of the average principal component revealed significant differences between the experimental sites. In comparison with the control site, the percentage of fatty acid biomarkers of Gram-positive bacteria was significantly higher in the contaminated areas, as well as the ratio of trans/cis isomerization in the case of 16:1ω7 and 18:1ω7 fatty acids. The inverse tendency was observed in the relative quantities of fatty acid biomarkers of Gram-negative bacteria compared to Actinomycetes, and in the fungal-bacterial ratio. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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15 pages, 3516 KiB  
Article
Convolutional Neural Network Applications in Fire Debris Classification
by Anuradha Akmeemana, Mary R. Williams and Michael E. Sigman
Chemosensors 2022, 10(10), 377; https://doi.org/10.3390/chemosensors10100377 - 21 Sep 2022
Viewed by 1781
Abstract
Convolutional neural networks (CNNs) are inspired by the visual cortex of the brain. In this work, CNNs, are applied to classify ground truth samples as positive or negative for ignitable liquid residue (ILR+ and ILR−, respectively). Known ground truth samples [...] Read more.
Convolutional neural networks (CNNs) are inspired by the visual cortex of the brain. In this work, CNNs, are applied to classify ground truth samples as positive or negative for ignitable liquid residue (ILR+ and ILR−, respectively). Known ground truth samples included laboratory-generated fire debris samples, neat ignitable liquids (ILs), single-substrate (SUB) burned samples and computationally generated (in silico) training samples. The images were generated from the total ion spectra for both training and test datasets by applying a wavelet transformation. The training set consisted of 50,000 in silico-generated fire debris samples. The probabilities generated from the CNN are used to calculate the likelihood ratios. These likelihood ratios were calibrated using logistic regression and the empirical cross-entropy (ECE) plots were used to investigate the calibration of the probabilities of the presence of ILRs (i.e., probability of belonging to class ILR+). The performance of the model was evaluated by the area under the receiver operating characteristic plots (ROC AUC). The ROC AUC for the laboratory-generated fire debris samples and the combined IL and SUB samples was 0.87 and 0.99, respectively. The CNNs trained on in silico data did significantly better predicting the classification of the pure IL (ILR+) and SUB (ILR−) samples. Nonetheless, the classification performance for laboratory-generated samples was sufficient to aid forensic analysts in the classification of casework samples. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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Review

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34 pages, 1619 KiB  
Review
New Applications of Gas Chromatography and Gas Chromatography-Mass Spectrometry for Novel Sample Matrices in the Forensic Sciences: A Literature Review
by Oliver Gould, Ngoc Nguyen and Kevin C. Honeychurch
Chemosensors 2023, 11(10), 527; https://doi.org/10.3390/chemosensors11100527 - 07 Oct 2023
Cited by 2 | Viewed by 3006
Abstract
The investigation of novel sample matrices in the forensic sciences offers several possible advantages, such as allowing for results to be obtained in cases where common sample types are absent. This review focuses on the application of gas chromatography and gas chromatography–mass spectrometry [...] Read more.
The investigation of novel sample matrices in the forensic sciences offers several possible advantages, such as allowing for results to be obtained in cases where common sample types are absent. This review focuses on the application of gas chromatography and gas chromatography–mass spectrometry (GC-MS) for the determination of drugs in alternative sample matrices, including hair, sweat, meconium, breast milk, and vitreous humour. Less common sample types are also reported including air, cerumen, insects, and their larvae and pupae. The application of pyrolysis GC-MS (Py GC-MS) is also reviewed, showing the possibility of determining high molecular weight drugs which would commonly be unattainable by GC-MS. The application of Py GC-MS for the simulation and investigation of the underlying chemistry and the products formed in the smoking of drugs is also reported. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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21 pages, 360 KiB  
Review
Modern Analytical Techniques for Berry Authentication
by Celia Carrillo, Igor B. Tomasevic, Francisco J. Barba and Senem Kamiloglu
Chemosensors 2023, 11(9), 500; https://doi.org/10.3390/chemosensors11090500 - 14 Sep 2023
Cited by 1 | Viewed by 1157
Abstract
The health-related properties attributed to berries and the subsequent interest awakened within the market of functional foods mean that these small fruits may be potential targets for food fraud. In this review, studies on berry authentication through modern analytical techniques are discussed in [...] Read more.
The health-related properties attributed to berries and the subsequent interest awakened within the market of functional foods mean that these small fruits may be potential targets for food fraud. In this review, studies on berry authentication through modern analytical techniques are discussed in detail. Most of the studies reported to date are related to chemical approaches, mainly chromatographic techniques. Other chemical (NMR, NIR, and Raman spectroscopy), biomolecular, and isotopic methods have also delivered promising results in the field of berry authentication, although there is still limited information available in this respect. Despite the potential of the methods described in the present review, to date, there is no universal one. Therefore, combinations of different approaches in order to complement each other are increasingly used (e.g., HPTLC and mass spectrometry; Raman and IR spectroscopies; biomolecular and analytical techniques…). Considering that adulteration practices are increasingly evolving, continuous research in the field of food authentication is needed, especially in the case of berries, since there are still some berry species that have not yet been included in any authentication study. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
18 pages, 1263 KiB  
Review
Total Ion Chromatogram and Total Ion Mass Spectrum as Alternative Tools for Detection and Discrimination (A Review)
by Marta Barea-Sepúlveda, Hugo Duarte, María José Aliaño-González, Anabela Romano and Bruno Medronho
Chemosensors 2022, 10(11), 465; https://doi.org/10.3390/chemosensors10110465 - 08 Nov 2022
Cited by 6 | Viewed by 3395
Abstract
Gas chromatography (GC) and mass spectrometry (MS) are widely used techniques in the analysis of complex mixtures due to their various advantages, such as high selectivity, reproducibility, precision, and sensitivity. However, the data processing is often complex and time-consuming and requires a great [...] Read more.
Gas chromatography (GC) and mass spectrometry (MS) are widely used techniques in the analysis of complex mixtures due to their various advantages, such as high selectivity, reproducibility, precision, and sensitivity. However, the data processing is often complex and time-consuming and requires a great deal of experience, which might be a serious drawback in certain areas, such as quality control, or regarding research in the field of medicine or forensic sciences, where time plays a crucial role. For these reasons, some authors have proposed the use of alternative data processing approaches, such as the total ion chromatogram or total mass spectrum, allowing these techniques to be treated as sensors where each retention time or ratio m/z acts as a sensor collecting total intensities. In this way, the main advantages associated with both techniques are maintained, but the outcomes from the analysis can be reached in a faster, simpler, and an almost automated way. In this review, the main features of the GC- and MS-based analysis methodologies and the ways in which to apply them are highlighted. Moreover, their implementation in different fields, such as agri-food, forensics, environmental sciences, or medicine is discussed, highlighting important advantages as well as limitations. Full article
(This article belongs to the Special Issue GC, MS and GC-MS Analytical Methods: Opportunities and Challenges)
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