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24 pages, 7104 KiB  
Review
Recent Advances in Metal Oxide Semiconductor Heterojunctions for the Detection of Volatile Organic Compounds
by Shengming Zhang, Heng Zhang, Haiyu Yao, Peijie Wang, Min Zhu, Xuerong Shi and Shusheng Xu
Chemosensors 2024, 12(12), 244; https://doi.org/10.3390/chemosensors12120244 - 22 Nov 2024
Viewed by 358
Abstract
The efficient detection of volatile organic compounds (VOCs) is critically important in the domains of environmental protection, healthcare, and industrial safety. The development of metal oxide semiconductor (MOS) heterojunction gas-sensing materials is considered one of the most effective strategies to enhance sensor performance. [...] Read more.
The efficient detection of volatile organic compounds (VOCs) is critically important in the domains of environmental protection, healthcare, and industrial safety. The development of metal oxide semiconductor (MOS) heterojunction gas-sensing materials is considered one of the most effective strategies to enhance sensor performance. This review summarizes and discusses the types of heterojunctions and their working principles, enhancement strategies, preparation methodologies, and applications in acetone and ethanol detection. To address the constraints pertaining to low sensitivity, sluggish response/recovery times, and elevated operating temperatures that are inherent in VOC sensors, several improvement methods are proposed, including doping with metals like Ag and Pd, incorporating additives such as MXene and polyoxometalates, optimizing morphologies through a fine design, and self-doping via oxygen vacancies. Furthermore, this work provides insights into the challenges faced by MOSs heterojunction-based gas sensors and outlines future research directions in this field. This review will contribute to foundational theories to overcome existing bottlenecks in MOS heterojunction technology while promoting its large-scale application in disease screening or agricultural food quality assessments. Full article
(This article belongs to the Special Issue Functional Nanomaterial-Based Gas Sensors and Humidity Sensors)
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<p>Illustration of three types of heterojunction.</p>
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<p>Illustration of strategies for promoting the sensing performance of MOS heterojunctions.</p>
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<p>Illustrations of preparation methods for MOSs heterojunction materials.</p>
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<p>(<b>a</b>) The TEM image of hierarchical Fe<sub>2</sub>O<sub>3</sub>-Co<sub>3</sub>O<sub>4</sub> heterojunction; (<b>b</b>) the contents of oxygen species based on the analysis of X-ray photoelectron spectroscopy (XPS); (<b>c</b>) the dynamic dot-line pattern of three sensors; (<b>d</b>) the selectivity of all gas sensors’ exposure to 100 ppm of different gases [<a href="#B86-chemosensors-12-00244" class="html-bibr">86</a>]. Reprinted with permission from Elsevier, copyright 2024.</p>
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<p>Schematic illustration of the synthetic process of the ZIF-67-derived oxide cage/nanofiber Co<sub>3</sub>O<sub>4</sub>/In<sub>2</sub>O<sub>3</sub> heterostructure for acetone gas sensing [<a href="#B55-chemosensors-12-00244" class="html-bibr">55</a>]. Reprinted with permission from [<a href="#B56-chemosensors-12-00244" class="html-bibr">56</a>]. Copyright {2024} American Chemical Society.</p>
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<p>(<b>a</b>) Illustration of the preparation process for the Ag-NiO/SnO<sub>2</sub> nanotubes (NTs); (<b>b</b>) scanning electron microscope (SEM) image; (<b>c</b>) transmission electron microscope (TEM) image; and (<b>d</b>) the diagram of the energy band structure of the Ag-NiO/SnO<sub>2</sub> NTs [<a href="#B87-chemosensors-12-00244" class="html-bibr">87</a>]. Reprinted with permission from Elsevier, copyright 2024. (<b>e</b>) Synthetic scheme of ZnO-CuO core–hollow cube nanostructures [<a href="#B90-chemosensors-12-00244" class="html-bibr">90</a>]. Reprinted with permission from [<a href="#B91-chemosensors-12-00244" class="html-bibr">91</a>]. Copyright {2020} American Chemical Society.</p>
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<p>(<b>a</b>) Preparation of the p-type CuO/TiO<sub>2</sub>/MXene gas-sensitive sensor; (<b>b</b>) energy band diagram of the gas-sensitive sensor in four different situations [<a href="#B102-chemosensors-12-00244" class="html-bibr">102</a>]. Reprinted with permission from [<a href="#B104-chemosensors-12-00244" class="html-bibr">104</a>]. Copyright {2024} American Chemical Society.</p>
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<p>(<b>a</b>) Schematic illustration of the formation process of the 3% Fe<sub>2</sub>O<sub>3</sub>-loaded ultrathin nanosheet assembled hollowed-out hierarchical NiO nanorods (Fe<sub>2</sub>O<sub>3</sub>@NiO); (<b>b</b>) SEM and TEM images of Fe<sub>2</sub>O<sub>3</sub>@NiO; (<b>c</b>) response of the Fe<sub>2</sub>O<sub>3</sub>@NiO to 10 ppm ethanol at different operating temperatures and 80% RH; (<b>d</b>) response of the Fe<sub>2</sub>O<sub>3</sub>@NiO at 150 °C to 10 ppm of different target gases under different humidity conditions [<a href="#B98-chemosensors-12-00244" class="html-bibr">98</a>]. Reprinted with permission from [<a href="#B99-chemosensors-12-00244" class="html-bibr">99</a>]. Copyright {2023} American Chemical Society.</p>
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<p>(<b>a</b>) The schematic illustration of the construction and engineering of SnO<sub>2</sub>-ZnO based on MOF precursor and corresponding TEM and HRTEM images [<a href="#B115-chemosensors-12-00244" class="html-bibr">115</a>]. Reprinted with permission from Elsevier, copyright 2023.; (<b>b</b>) SEM image of ZnO-SnO<sub>2</sub> heterojunction IOPBs; and (<b>c</b>) the response at 260 °C to 10, 20, 50, 80, and 100 ppm acetone [<a href="#B69-chemosensors-12-00244" class="html-bibr">69</a>]. Reprinted with permission from Elsevier, copyright 2024.</p>
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<p>Schematic diagram of gas molecular adsorption, electron transfer, and energy band structure for the In<sub>2</sub>O<sub>3</sub>-ZnO material in (<b>a</b>) air and (<b>b</b>) ethanol [<a href="#B50-chemosensors-12-00244" class="html-bibr">50</a>]. Reprinted with permission from Elsevier, copyright 2023.</p>
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<p>(<b>a</b>) SEM image of Zn<sub>2</sub>SnO<sub>4</sub>/CdSnO<sub>3</sub>; (<b>b</b>) EPR spectra of CdSnO<sub>3</sub>, Zn<sub>2</sub>SnO<sub>4</sub>, and Zn<sub>2</sub>SnO<sub>4</sub>/CdSnO<sub>3</sub>; (<b>c</b>) schematic diagram of the energy band structure and ethanol gas sensing process of CdSnO<sub>3</sub>/Zn<sub>2</sub>SnO<sub>4</sub> heterostructure [<a href="#B57-chemosensors-12-00244" class="html-bibr">57</a>]. Reprinted with permission from Elsevier, copyright 2024.</p>
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<p>(<b>a</b>) Schematic illustration of the fabrication process of In<sub>2</sub>O<sub>3</sub>@PW<sub>12</sub>@SnO<sub>2</sub> NFs [<a href="#B97-chemosensors-12-00244" class="html-bibr">97</a>]; (<b>b</b>) TEM image of In@3%P@Sn NFs after calcination and selectivity pattern of the gas sensors based on In@3%P@Sn [<a href="#B97-chemosensors-12-00244" class="html-bibr">97</a>]; (<b>c</b>) transient responses of different concentrations of ethanol at the optimal operating temperature [<a href="#B97-chemosensors-12-00244" class="html-bibr">97</a>]. Reprinted with permission from Elsevier, copyright 2024.</p>
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<p>(<b>a</b>) Formation process schematic for SnO<sub>2</sub>/ZnO/Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> MXene nanocomposites; (<b>b</b>) the curves for dynamic response and recovery of SnO<sub>2</sub>/ZnO/Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> MXene at 120 °C to 100 ppm ethanol [<a href="#B103-chemosensors-12-00244" class="html-bibr">103</a>]; (<b>c</b>) SnO<sub>2</sub>/ZnO/Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> MXene responses to various gases (100 ppm) at 120 °C [<a href="#B103-chemosensors-12-00244" class="html-bibr">103</a>]; (<b>d</b>) electron transfer of ZnO, SnO<sub>2</sub>, and Ti<sub>3</sub>C<sub>2</sub>T<sub>x</sub> MXene in air and ethanol [<a href="#B103-chemosensors-12-00244" class="html-bibr">103</a>]. Reprinted with permission from Elsevier, copyright 2024.</p>
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21 pages, 7736 KiB  
Article
Carbonyl Compounds Observed at a Suburban Site during an Unusual Wintertime Ozone Pollution Event in Guangzhou
by Aoqi Ge, Zhenfeng Wu, Shaoxuan Xiao, Xiaoqing Huang, Wei Song, Zhou Zhang, Yanli Zhang and Xinming Wang
Atmosphere 2024, 15(10), 1235; https://doi.org/10.3390/atmos15101235 - 16 Oct 2024
Viewed by 530
Abstract
Carbonyl compounds are important oxygenated volatile organic compounds (VOCs) that play significant roles in the formation of ozone (O3) and atmospheric chemistry. This study presents comprehensive field observations of carbonyl compounds during an unusual wintertime ozone pollution event at a suburban [...] Read more.
Carbonyl compounds are important oxygenated volatile organic compounds (VOCs) that play significant roles in the formation of ozone (O3) and atmospheric chemistry. This study presents comprehensive field observations of carbonyl compounds during an unusual wintertime ozone pollution event at a suburban site in Guangzhou, South China, from 19 to 28 December 2020. The aim was to investigate the characteristics and sources of carbonyls, as well as their contributions to O3 formation. Formaldehyde, acetone, and acetaldehyde were the most abundant carbonyls detected, with average concentrations of 7.11 ± 1.80, 5.21 ± 1.13, and 3.00 ± 0.94 ppbv, respectively, on pollution days, significantly higher than those of 2.57 ± 1.12, 2.73 ± 0.88, and 1.10 ± 0.48 ppbv, respectively, on nonpollution days. The Frame for 0-D Atmospheric Modeling (F0AM) box model simulations revealed that local production accounted for 62–88% of observed O3 concentrations during the pollution days. The calculated ozone formation potentials (OFPs) for various precursors (carbonyls and VOCs) indicated that carbonyl compounds contributed 32.87% of the total OFPs on nonpollution days and 36.71% on pollution days, respectively. Formaldehyde, acetaldehyde, and methylglyoxal were identified as the most reactive carbonyls, and formaldehyde ranked top in OFPs, and it alone contributed 15.92% of total OFPs on nonpollution days and 18.10% of total OFPs on pollution days, respectively. The calculation of relative incremental reactivity (RIR) indicates that ozone sensitivity was a VOC-limited regime, and carbonyls showed greater RIRs than other groups of VOCs. The model simulation showed that secondary formation has a significant impact on formaldehyde production, which is primarily controlled by alkenes and biogenic VOCs. The characteristic ratios and backward trajectory analysis also indicated the indispensable impacts of local primary sources (like industrial emissions and vehicle emissions) and regional sources (like biomass burning) through transportation. This study highlights the important roles of carbonyls, particularly formaldehyde, in forming ozone pollution in megacities like the Pearl River Delta region. Full article
(This article belongs to the Section Air Quality)
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<p>Location of the observation site (green star).</p>
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<p>Time series of meteorological parameters and major pollutants during the sampling period, with shaded areas indicating the pollution days.</p>
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<p>Diurnal variations of major carbonyls during pollution days and nonpollution days.</p>
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<p>The contributions of different VOC groups to ozone formation potential (OFP) during the nonpollution and pollution days.</p>
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<p>Carbonyls and NMHC compounds with the top 10 OFP values during nonpollution and pollution days.</p>
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<p>Model simulation of O<sub>3</sub> formation.</p>
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<p>Calculated RIRs for ozone formation from precursors (carbonyls, NMHCs, and NOx).</p>
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<p>Observed and simulated concentrations of formaldehyde during the sampling period.</p>
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<p>Model-simulated production rate (P (HCHO)) and loss rate (L (HCHO)) of formaldehyde through different reaction pathways during nonpollution days (<b>a</b>) and pollution days (<b>b</b>).</p>
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<p>The calculated RIRs of the five major HC groups for the formation of formaldehyde.</p>
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<p>Model-calculated RIRs of the individual top 10 NMHC species for the formation of formaldehyde during pollution days.</p>
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<p>Correlation analysis of formaldehyde to acetaldehyde (<b>a</b>), acetaldehyde to propanal (<b>b</b>), toluene to benzene (<b>c</b>), and m,p-xylene to ethylbenzene (<b>d</b>) during nonpollution days and pollution days.</p>
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<p>Mean 48 h back trajectories of clusters at the Huadu site (black star) during nonpollution days (<b>a</b>) and pollution days (<b>b</b>).</p>
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<p>Backward trajectory and fire hotspot map within 48 h during the sampling period from 19 to 28 December 2020 (24 trajectories per day) at the Huadu site (black star).</p>
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14 pages, 9126 KiB  
Article
Acetone Sensors Based on Al-Coated and Ni-Doped Copper Oxide Nanocrystalline Thin Films
by Dinu Litra, Maxim Chiriac, Nicolai Ababii and Oleg Lupan
Sensors 2024, 24(20), 6550; https://doi.org/10.3390/s24206550 - 11 Oct 2024
Viewed by 690
Abstract
Acetone detection is of significant importance in various industries, from cosmetics to pharmaceuticals, bioengineering, and paints. Sensor manufacturing involves the use of different semiconductor materials as well as different metals for doping and functionalization, allowing them to achieve advanced or unique properties in [...] Read more.
Acetone detection is of significant importance in various industries, from cosmetics to pharmaceuticals, bioengineering, and paints. Sensor manufacturing involves the use of different semiconductor materials as well as different metals for doping and functionalization, allowing them to achieve advanced or unique properties in different sensor applications. In the healthcare field, these sensors play a crucial role in the non-invasive diagnosis of various diseases, offering a potential way to monitor metabolic conditions by analyzing respiration. This article presents the synthesis method, using chemical solutions and rapid thermal annealing technology, to obtain Al-functionalized and Ni-doped copper oxide (Al/CuO:Ni) nanostructured thin films for biosensors. The nanocrystalline thin films are subjected to a thorough characterization, with examination of the morphological properties by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD) analysis. The results reveal notable changes in the surface morphology and structure following different treatments, providing insight into the mechanism of function and selectivity of these nanostructures for gases and volatile compounds. The study highlights the high selectivity of developed Al/CuO:Ni nanostructures towards acetone vapors at different concentrations from 1 ppm to 1000 ppm. Gas sensitivity is evaluated over a range of operating temperatures, indicating optimum performance at 300 °C and 350 °C with the maximum sensor signal (S) response obtained being 45% and 50%, respectively, to 50 ppm gas concentration. This work shows the high potential of developed technology for obtaining Al/CuO:Ni nanostructured thin films as next-generation materials for improving the sensitivity and selectivity of acetone sensors for practical applications as breath detectors in biomedical diagnostics, in particular for diabetes monitoring. It also emphasizes the importance of these sensors in ensuring industrial safety by preventing adverse health and environmental effects of exposure to acetone. Full article
(This article belongs to the Section Nanosensors)
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<p>Graphical representation of the use of acetone sensors in different fields.</p>
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<p>The proposed concept of acetone vapor detection in exhaled air using an oxide-based sensor structure.</p>
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<p>SEM images of CuO:Ni nanostructures: (<b>a</b>) before RTA treatment at a scale of 400 nm, (<b>b</b>) after RTA treatment (600 °C for 30 s in air) at a scale of 400 nm, and (<b>c</b>) after RTA treatment at a scale of 100 nm. SEM images after functionalization with Al and thermal annealing at a scale of (<b>d</b>) 2 μm and (<b>e</b>) 400 nm, respectively.</p>
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<p>(<b>a</b>) XRD patterns in the range of 30–45 degrees of CuO:Ni thin films as grown and RTA-treated at 600 °C for 30 s in air and (<b>b</b>) XRD pattern in the range of 30–80 degrees of CuO:Ni after RTA treatment at 600 °C for 30 s in air.</p>
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<p>The response of Al-functionalized and Ni-doped copper oxide nanocrystalline thin films to acetone, methane, ammonia, 2-propanol, and carbon dioxide gases with a concentration of 50 ppm.</p>
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<p>The dynamic response to acetone vapor of Al/CuO:Ni nanostructured film-based sensor at 350 °C at concentrations of: (<b>a</b>) 1 ppm, 5 ppm, and 10 ppm and (<b>b</b>) 50 ppm, 100 ppm, 500 ppm, and 1000 ppm.</p>
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<p>The dynamic response to acetone vapor of Al/CuO:Ni nanostructured film-based sensor at 350 °C at concentrations of: (<b>a</b>) 1 ppm, 5 ppm, and 10 ppm and (<b>b</b>) 50 ppm, 100 ppm, 500 ppm, and 1000 ppm.</p>
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<p>(<b>a</b>) Gas response as a function of acetone vapor concentrations for Al/CuO:Ni structure-based sensors at operating temperature of 350 °C. (<b>b</b>) Dynamic response at operating temperature of 350 °C of Al/CuO:Ni structure-based sensor to acetone vapor concentrations of 1 ppm, 5 ppm, and 100 ppm.</p>
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<p>Schematic representation of the Al/CuO:Ni structure (<b>a</b>) in air and (<b>b</b>) in acetone vapors. Schematic representation of the corresponding energy bands (<b>c</b>) in air and (<b>d</b>) in acetone vapors.</p>
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10 pages, 1635 KiB  
Article
Associations between Kidney Disease Progression and Metabolomic Profiling in Stable Kidney Transplant Recipients—A 3 Year Follow-Up Prospective Study
by Titus Andrian, Lucian Siriteanu, Luminița Voroneanu, Alina Nicolescu, Calin Deleanu, Andreea Covic and Adrian Covic
J. Clin. Med. 2024, 13(19), 5983; https://doi.org/10.3390/jcm13195983 - 8 Oct 2024
Viewed by 690
Abstract
Background: kidney transplant recipients are exposed to multiple pathogenic pathways that may alter short and long-term allograft survival. Metabolomic profiling is useful for detecting potential biomarkers of kidney disease with a predictive capacity. This field is still under development in kidney transplantation and [...] Read more.
Background: kidney transplant recipients are exposed to multiple pathogenic pathways that may alter short and long-term allograft survival. Metabolomic profiling is useful for detecting potential biomarkers of kidney disease with a predictive capacity. This field is still under development in kidney transplantation and metabolome analysis is faced with analytical challenges. We performed a cross-sectional study including stable kidney transplant patients and aimed to search for relevant associations between baseline plasmatic and urinary metabolites and relevant outcomes over a follow-up period of 3 years. Methods: we performed a cross-sectional study including 72 stable kidney transplant patients with stored plasmatic and urinary samples at the baseline evaluation which were there analyzed by nuclear magnetic resonance in order to quantify and describe metabolites. We performed a 3-year follow-up and searched for relevant associations between renal failure outcomes and baseline metabolites. Between-group comparisons were made after classification by observed estimated glomerular filtration rate slope during the follow-up: positive slope and negative slope. Results: The mean estimated GFR (glomerular filtration rate) was higher at baseline in the patients who exhibited a negative slope during the follow-up (63.4 mL/min/1.73 m2 vs. 55.8 mL/min/1.73 m2, p = 0,019). After log transformation and division by urinary creatinine, urinary dimethylamine (3.63 vs. 3.16, p = 0.027), hippuric acid (7.33 vs. 6.29, p = 0.041), and acetone (1.88 vs. 1, p = 0.023) exhibited higher concentrations in patients with a negative GFR slope when compared to patients with a positive GFR slope. By computing a linear regression, a significant low-strength regression equation between the log 2 transformed plasmatic level of glycine and the estimated glomerular filtration rate was found (F (1,70) = 5.15, p = 0.026), with an R2 of 0.069. Several metabolites were correlated positively with hand grip strength (plasmatic tyrosine with r = 0.336 and p = 0.005 and plasmatic leucine with r = 0.371 and p = 0.002). Other urinary metabolites were found to be correlated negatively with hand grip strength (dimethylamine with r = −0.250 and p = 0.04, citric acid with r = −0.296 and p = 0.014, formic acid with r = −0.349 and p = 0.004, and glycine with r = −0.306 and p = 0.01). Conclusions: some metabolites had different concentrations compared to kidney transplant patients with negative and positive slopes, and significant correlations were found between hand grip strength and urinary and plasmatic metabolites. Full article
(This article belongs to the Special Issue Clinical Advancements in Kidney Transplantation)
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<p>Significant differences in urinary metabolites in kidney transplant recipients with different GFR slope trajectories.</p>
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<p>Significant differences in plasmatic metabolites in kidney transplant recipients with different GFR slope trajectories.</p>
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<p>Significant linear relationship between plasmatic Glycine and estimated GFR.</p>
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<p>Correlation plots of statistically significant Pearson’s correlation among quantified metabolites (all log 2 transformed) with each other and with hand grip strength.</p>
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11 pages, 1191 KiB  
Article
Breath Analysis via Gas Chromatography–Mass Spectrometry (GC-MS) in Chronic Coronary Syndrome (CCS): A Proof-of-Concept Study
by Marco Lombardi, Andrea Segreti, Marco Miglionico, Giorgio Pennazza, Lorenzo Tocca, Luca Amendola, Rocco Vergallo, Germano Di Sciascio, Italo Porto, Francesco Grigioni and Raffaele Antonelli Incalzi
J. Clin. Med. 2024, 13(19), 5857; https://doi.org/10.3390/jcm13195857 - 1 Oct 2024
Viewed by 823
Abstract
Background: This proof-of-concept study aimed to assess the diagnostic potential of gas chromatography–mass spectrometry (GC-MS) in profiling volatile organic compounds (VOCs) from exhaled breath as a diagnostic tool for the chronic coronary syndrome (CCS). Methods: Exhaled air was collected from patients undergoing invasive [...] Read more.
Background: This proof-of-concept study aimed to assess the diagnostic potential of gas chromatography–mass spectrometry (GC-MS) in profiling volatile organic compounds (VOCs) from exhaled breath as a diagnostic tool for the chronic coronary syndrome (CCS). Methods: Exhaled air was collected from patients undergoing invasive coronary angiography (ICA), with all samples obtained prior to ICA. Post hoc, patients were divided into groups based on coronary lesion severity and indications for revascularization. VOCs in the breath samples were analyzed using GC-MS. Results: This study included 23 patients, of whom 11 did not require myocardial revascularization and 12 did. GC-MS analysis successfully classified 10 of the 11 patients without the need for revascularization (sensitivity of 91%), and 7 of the 12 patients required revascularization (specificity 58%). In subgroup analysis, GC-MS demonstrated 100% sensitivity in identifying patients with significant coronary lesions requiring intervention when the cohort was divided into three groups. A total of 36 VOCs, including acetone, ethanol, and phenol, were identified as distinguishing markers between patient groups. Conclusions: Patients with CCS exhibited a unique fingerprint of exhaled breath, which was detectable with GC-MS. These findings suggest that GC-MS analysis could be a reliable and non-invasive diagnostic tool for CCS. Further studies with larger cohorts are necessary to validate these results and explore the potential integration of VOC analysis into clinical practice. Full article
(This article belongs to the Section Cardiology)
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<p>Exhaled air collection. Each patient provided a single sample by breathing tidally for three minutes into a dedicated storage device equipped with an adsorbing cartridge (Pneumopipe<sup>®</sup>). This device captures volatile organic compounds (VOCs) from the exhaled air for subsequent analysis using gas chromatography–mass spectrometry (GC-MS).</p>
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<p>Exhaled breath collection and analysis. Each patient provided a single breath sample into a Pneumopipe<sup>®</sup> device containing an adsorbing cartridge. Volatile organic compounds (VOCs) from Tenax cartridges were collected in 500 mL Tedlar bags and analyzed using the carboxen solid phase microextraction (SPME) gas chromatography–mass spectrometry (GC-MS) technique. The SPME fiber was thermally desorbed in the GC injector at 280 °C. Data were derived from GC-MS chromatogram analysis, expressed as the ratio of the VOC area to the reference peak area, and analyzed using a partial least square discriminant analysis (PLS-DA) model.</p>
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<p>Experimental timeline of the study. Patients with suspected chronic coronary syndrome and a clinical indication for invasive coronary angiography (ICA) admitted to the Cardiology Unit of Campus Bio-Medico Hospital of Rome were enrolled in this study. A total of 23 patients were included. Exhaled breath collection and GC-MS analysis were performed before ICA. Based on the ICA findings, the population was divided into two groups: 11 subjects who did not require myocardial revascularization and 12 patients who required myocardial revascularization.</p>
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<p>Graphical representation of data derived from gas chromatography–mass spectrometry (GC-MS) analysis. The results are expressed as the ratio of the VOCs’ area to the reference peak area on the y-axis, while the x-axis displays the VOCs detected in exhaled breath using GC-MS. The plot shows the distribution of VOCs from a patient included in the study who underwent revascularization. The red line represents the patient’s breath analysis, while the black line represents the control sample used for comparison.</p>
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10 pages, 7573 KiB  
Communication
Rapid Purification and Quantification of Intestinal and Fecal Short-Chain Fatty Acids by Solid-Phase Extraction Using Bond Elut Plexa
by Xing Zheng, Tao Chen, Wanli Li, Kai Wang, Xiaofeng Xue, Nenad Naumovski and Wenjun Peng
Separations 2024, 11(9), 270; https://doi.org/10.3390/separations11090270 - 16 Sep 2024
Viewed by 955
Abstract
Short-chain fatty acids (SCFAs) in feces are inextricably linked to intestinal homeostasis and can be used as potential markers for metabolic diseases. In this study, an efficient and simple method was developed for the purification of SCFAs without the need for derivatization of [...] Read more.
Short-chain fatty acids (SCFAs) in feces are inextricably linked to intestinal homeostasis and can be used as potential markers for metabolic diseases. In this study, an efficient and simple method was developed for the purification of SCFAs without the need for derivatization of the samples. The SCFAs (acetic, propionic, isobutyric, butyric, isovaleric, valeric, and hexanoic acid) were extracted from a small amount (50 mg) of fecal and intestinal samples using acetone combined with solid phase extraction column (Bond Elut Plexa) enrichment. Quantitative analysis was performed using gas chromatography with a flame ionization detector. The developed method has shown very good limits of detection (LOD, 0.11–0.36 μM) and limits of quantification (LOQ, 0.38–1.21 μM) with excellent linearity (R2 ≥ 0.9998), good recovery (98.34–137.83%), and high reproducibility (RSD ≤ 1.30). The applicability of this method was also demonstrated by testing the fecal and cecum contents of different species from mammals (mice, pigs) to insects (honeybees). The technique is highly suitable for analyzing complex, small amounts of intestinal and fecal SCFAs. Full article
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<p>Flow chart and theory of extracting SCFA from fecal samples.</p>
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<p>Chromatogram of mixed standards at L3 concentration (representing the average physiological concentration of SCFAs in the fecal and intestinal samples). Acetic acid, 107.41 µM; Propionic acid, 80.32 µM; Isobutyric acid, 63.11 µM; Butyric acid 64.92 µM; Isovaleric acid, 53.56 µM; Valeric acid, 54.34 µM; Hexanoic acid, 45.89 µM.</p>
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<p>(<b>A</b>) Gas chromatograms of standards and samples. (a) SCFA standards of L3 concentration; (b) SCFA extract from mouse cecum contents; (c) SCFA extract from mouse feces; (d) SCFA extract from pig cecum contents; (e) SCFA extract from pig feces; (f) SCFA extract from honeybees’ (Apis mellifera) intestinal contents. Numbers 1−7 represent acetic, propionic, isobutyric, butyric, isovaleric, valeric and hexanoic acid, respectively. (<b>B</b>) The PCA plots of the SCFA data in fecal and intestinal content samples from different sources. MCC, mouse cecum contents; MF, mouse feces; PCC, pig cecum contents; PF, pig feces; HIC, honeybee intestinal contents. (<b>C</b>) To compare the levels of acetic, propionic, isobutyric, butyric, isovaleric, valeric, and hexanoic acids in different samples. Statistical data are expressed as mean ± standard deviation. The results corresponding to bars with different letters were statistically significant (<span class="html-italic">p</span> &lt; 0.05). On the contrary, the results corresponding to bars with the same letter were not statistically significant.</p>
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16 pages, 2235 KiB  
Article
Effect of Flammulina velutipes Soluble Dietary Fiber on Dough Processing Characteristics and Micro-Fermented Dried Noodles Quality Properties
by Wenliang Wang, Shuang Yang, Lihong Wang, Furong Hou, Shasha Song, Yansheng Wang, Zhiqing Gong and Fengjuan Jia
Foods 2024, 13(17), 2764; https://doi.org/10.3390/foods13172764 - 30 Aug 2024
Viewed by 767
Abstract
Our research focused on the integration of Flammulina velutipes soluble dietary fiber (Fv-SDF) into wheat flour during the production of dried noodles, delving into the impact of different addition ratios of Fv-SDF on both dough processing characteristics and the quality of the micro-fermented [...] Read more.
Our research focused on the integration of Flammulina velutipes soluble dietary fiber (Fv-SDF) into wheat flour during the production of dried noodles, delving into the impact of different addition ratios of Fv-SDF on both dough processing characteristics and the quality of the micro-fermented dried noodles. The viscometric and thermodynamic analyses revealed that Fv-SDF notably improved the thermal stability of the mix powder, reduced viscosity, and delayed starch aging. Additionally, Fv-SDF elevated the gelatinization temperature and enthalpy value of the blend. Farinograph Properties and dynamic rheology properties further indicated that Fv-SDF improved dough formation time, stability time, powder quality index, and viscoelasticity. Notably, at a 10% Fv-SDF addition, the noodles achieved the highest sensory score (92) and water absorption rate (148%), while maintaining a lower dry matter loss rate (5.2%) and optimal cooking time (142 s). Gas chromatography-ion mobility spectrometry (GC-IMS) analysis showed that 67 volatile substances were detected, and the contents of furfural, 1-hydroxy-2-acetone, propionic acid, and 3-methylbutyraldehyde were higher in the Fv-SDF 10% group. These 10% Fv-SDF micro-fermented noodles were not only nutritionally enhanced, but also had a unique flavor. This study provides a valuable theoretical basis for the industrial application of F. velutipes and the development of high-quality dried noodles rich in Fv-SDF. Full article
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<p>Effect of Fv-SDF addition on the thermodynamic properties of wheat starch.</p>
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<p>Effect of Fv-SDF addition on the pasting properties of wheat starch.</p>
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<p>Effects of Fv-SDF addition on the storage modulus (G′) (<b>A</b>), loss modulus (G″) (<b>B</b>), and loss tangent (tanδ = G″/G′) (<b>C</b>) of dough.</p>
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<p>The effect of Fv-SDF addition on the optimum cooking time (<b>A</b>), water absorption, and cooking loss rate (<b>B</b>) of dried noodles. Different letters represent significance (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Effects of Fv-SDF addition on sensory evaluation of dried noodles. Different letters represent significance (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Three-dimensional spectrum of volatile substance composition (<b>A</b>), 2D spectrum of volatile substance composition (<b>B</b>), 2D differential spectrum of volatile substance composition (<b>C</b>), GC-IMS fingerprint (<b>D</b>), PCA analysis (<b>E</b>). In (<b>A</b>–<b>C</b>), the samples from left to right are the CK group, Fv-SDF 0% group, and Fv-SDF 10% group, respectively.</p>
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13 pages, 1117 KiB  
Article
Phytochemistry of Argemone ochroleuca Sweet Extracts and Their Inhibitory Effects on Maize Seed Germination
by Nezelo T. Mlombo, Zakheleni P. Dube, Fikile N. Makhubu and Hellen Nxumalo
Agronomy 2024, 14(9), 1912; https://doi.org/10.3390/agronomy14091912 - 26 Aug 2024
Viewed by 589
Abstract
Argemone ochroleuca Sweet is an alien invasive weed dominating most cultivated lands, however, the phytochemicals present in this plant and the effects of these on the germination and growth of economically important crops such as maize are not well-documented. The objective of the [...] Read more.
Argemone ochroleuca Sweet is an alien invasive weed dominating most cultivated lands, however, the phytochemicals present in this plant and the effects of these on the germination and growth of economically important crops such as maize are not well-documented. The objective of the study was to characterize the phytochemistry of the shoots and roots of A. ochroleuca and determine whether the extracts could inhibit the germination of maize seeds. The shoots and roots of A. ochroleuca were extracted in water, hexane, and acetone. Ten maize seeds were used in the germination bioassay. A phytochemical analysis was conducted using gas chromatography-mass spectrometry (GC-MS). The effects of the A. ochroleuca water, hexane, or acetone extracts on maize seed germination were concentration and plant-part dependent. The highest reduction was recorded from the water extract with 82%. Identified compounds with high percentages in A. ochroleuca were 9,12-octadecadienoic acid (Z,Z) and 9,12,15-octadecatrienoic acid, (Z,Z,Z)-. The present study indicated that A. ochroleuca extracts suppress the germination of maize seeds, likely due to the presence of both the identified and potentially unidentified phytochemicals that were not detected by the selected method. There is, however, a need to establish the relationship between the phytochemical compounds and the enzymes responsible for germination. Full article
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<p>Phytotoxic effects of the <span class="html-italic">Argemone ochroleuca</span> acetone extracts on the maize germination percentage.</p>
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<p>Phytotoxic effects of the <span class="html-italic">Argemone ochroleuca</span> acetone extracts on the maize radicle length.</p>
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<p>Effect of <span class="html-italic">Argemone ochroleuca</span> acetone extracts on the maize plumule length (mm).</p>
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14 pages, 2728 KiB  
Article
Organophosphate Detection in Animal-Derived Foods Using a Modified Quick, Easy, Cheap, Effective, Rugged, and Safe Method with Liquid Chromatography–Mass Spectrometry
by Byung-Joon Kim, Seung-Hyun Yang and Hoon Choi
Foods 2024, 13(16), 2642; https://doi.org/10.3390/foods13162642 - 22 Aug 2024
Viewed by 949
Abstract
Organophosphates are widely used in the livestock industry. In this study, we developed a method for detecting 27 organophosphate insecticides in animal-derived foods, including beef, pork, chicken, milk, and eggs, using liquid chromatography–tandem mass spectrometry. A modified QuEChERS method was optimized for sample [...] Read more.
Organophosphates are widely used in the livestock industry. In this study, we developed a method for detecting 27 organophosphate insecticides in animal-derived foods, including beef, pork, chicken, milk, and eggs, using liquid chromatography–tandem mass spectrometry. A modified QuEChERS method was optimized for sample pretreatment. A mixture of acetonitrile and acetone was used as the extraction solvent, and MgSO4 and NaCl were used as salts. Among the five different dispersive solid-phase extraction systems, MgSO4, primary secondary amines, and C18 were selected for purification because they had the highest recovery rates and least matrix effects. The matrix-dependent limit of quantitation was 0.0005–0.005 mg/kg, and the correlation coefficient of the matrix-matched calibration curve was >0.99, which was acceptable for quantifying residues below 0.01 mg/kg—the default maximum residue limit in a positive list system. The recovery efficiencies ranged from 71.9 to 110.5%, with standard deviations ranging from 0.2% to 12.5%, satisfying the SANTE guidelines. The established analytical method was used to monitor organophosphates in animal-derived foods obtained from a local market, and no pesticides were detected. With respect to industry standards, our proposed method is recommended for practical organophosphate detection in animal-derived foods. Full article
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<p>Comparison of LC–MS/MS chromatograms for organophosphates (200 µg/L) obtained from different columns: (<b>a</b>) UK-C18, (<b>b</b>) Kinetex-C18, (<b>c</b>) Xbridge-C18, and (<b>d</b>) Cardenza-C18.</p>
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<p>Extraction efficiencies of organophosphates in (<b>a</b>) eggs and (<b>b</b>) pork using various extraction solvents: acetone (ACE), acetonitrile (MeCN), and ACE/MeCN (5:5, <span class="html-italic">v</span>/<span class="html-italic">v</span>). The numbers (#1–#27) correspond to the organophosphates are listed in <a href="#foods-13-02642-t001" class="html-table">Table 1</a>. The dashed lines indicate a recovery threshold of 70%.</p>
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<p>Recovery rate of organophosphates in (<b>a</b>) eggs and (<b>b</b>) pork following purification with different d-SPE systems: d-SPE #1 (150 mg MgSO<sub>4</sub> and 25 mg PSA); d-SPE #2 (150 mg MgSO<sub>4</sub>, 25 mg PSA, and 25 mg C18); d-SPE #3 (150 mg MgSO<sub>4</sub> and 25 mg C18); d-SPE #4 (150 mg MgSO<sub>4</sub>, 25 mg PSA, and 25 mg GCB); and d-SPE #5 (150 mg MgSO<sub>4</sub> and 25 mg Z-sep).</p>
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<p>Impact of d-SPE on matrix effects of organophosphates in animal-derived foods. (<b>a</b>) beef, (<b>b</b>) pork, (<b>c</b>) chicken, (<b>d</b>) milk, and (<b>e</b>) eggs. The d-SPE systems are as follows. d-SPE #1: 150 mg MgSO<sub>4</sub> and 25 mg PSA; d-SPE #2: 150 mg MgSO<sub>4</sub>, 25 mg PSA, and 25 mg C18; d-SPE #3: 150 mg MgSO<sub>4</sub> and 25 mg C18.</p>
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<p>Impact of d-SPE on matrix effects of organophosphates in animal-derived foods. (<b>a</b>) beef, (<b>b</b>) pork, (<b>c</b>) chicken, (<b>d</b>) milk, and (<b>e</b>) eggs. The d-SPE systems are as follows. d-SPE #1: 150 mg MgSO<sub>4</sub> and 25 mg PSA; d-SPE #2: 150 mg MgSO<sub>4</sub>, 25 mg PSA, and 25 mg C18; d-SPE #3: 150 mg MgSO<sub>4</sub> and 25 mg C18.</p>
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12 pages, 1892 KiB  
Article
Comparison between Electropolymers of 3,5-Dihydroxybenzoic Acid and 2′,6′-Dihydroxyacetophenone in Dimethyl Sulfoxide and Their Analytical Performance towards Selected Analytes with the Role of the Washing Liquid
by László Kiss, Heng Li, Hui Yan and Sándor Kunsági-Máté
Molecules 2024, 29(16), 3972; https://doi.org/10.3390/molecules29163972 - 22 Aug 2024
Viewed by 557
Abstract
In the first part of this study, the electrochemical polymerization of two compounds, 3,5-dihydroxybenzoic acid and 2′,6′-dihydroxyacetophenone, was compared in dimethyl sulfoxide solvent on platinum and glassy carbon electrodes. The voltammograms obtained showed remarkable differences between the two monomers and between the two [...] Read more.
In the first part of this study, the electrochemical polymerization of two compounds, 3,5-dihydroxybenzoic acid and 2′,6′-dihydroxyacetophenone, was compared in dimethyl sulfoxide solvent on platinum and glassy carbon electrodes. The voltammograms obtained showed remarkable differences between the two monomers and between the two electrode materials. The acetophenone derivative formed electropolymer remnants at the electrodes, while in the case of the benzoic acid derivative, practically no passivation occurred, and the scanning electron microscopic results reinforced this. A few stackings adsorbed only after electropolymerization from a highly concentrated solution of dihydroxybenzoic acid. As a modifying layer on the platinum and glassy carbon electrodes, the prepared films from 2′,6′-dihydroxyacetophenone were tested for tributylamine in acetonitrile and in an aqueous solution of a redox-active compound, hydroquinone, during the stirring of the solution. More stable amperometric current signals could be reached with modified platinum than with glassy carbon, and the significant influence of the organic washing liquid after deposition was established via the study of noise level. In this respect, acetone was the best choice. The amperometric signals with the modified platinum obtained upon the addition of aliquots of the stock solution resulted in a 3.29 μM detection limit. Full article
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<p>Cyclic voltammograms for 3,5−dihydroxybenzoic acid (<b>a</b>) and 2′,6′−dihydroxyacetophenone (<b>b</b>) in dimethyl sulfoxide in their 100 mM solutions on a platinum electrode; (<b>c</b>) the same for 3,5−dihydroxybenzoic acid and (<b>d</b>) for 2′,6′−dihydroxybenzoic acid on a glassy carbon electrode (scan rate 0.1 V/s, supporting electrolyte 100 mM TBAP; the inset graphs show curves recorded in 25 mM solutions and the direction of arrows on curves indicate the direction of the change in voltametric peak heights).</p>
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<p>Scanning electron micrographs of electrodeposited films of 3,5-dihydroxybenzoic acid (35 Bz COOH, (<b>a</b>–<b>d</b>) and 2′,6′-dihydroxyacetophenone (26 acf, (<b>e</b>–<b>h</b>)) from dimethyl sulfoxide of different concentrations. The second numbers in labels reflect the monomer concentrations: (<b>a</b>–<b>d</b>) or (<b>e</b>–<b>h</b>) related to the 25 mM, 50 mM, 75 mM and 100 mM monomer concentrations, respectively.</p>
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<p>Scanning electron micrographs of electrodeposited films of 3,5-dihydroxybenzoic acid (35 Bz COOH, (<b>a</b>–<b>d</b>) and 2′,6′-dihydroxyacetophenone (26 acf, (<b>e</b>–<b>h</b>)) from dimethyl sulfoxide of different concentrations. The second numbers in labels reflect the monomer concentrations: (<b>a</b>–<b>d</b>) or (<b>e</b>–<b>h</b>) related to the 25 mM, 50 mM, 75 mM and 100 mM monomer concentrations, respectively.</p>
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<p>The dependence of the first peak currents on the concentration of 3,5-dihydroxybenzoic acid by varying the acetonitrile (ACN) content in <span class="html-italic">v</span>/<span class="html-italic">v</span> %.</p>
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<p>The dependence of peak currents (<b>a</b>) and peak potentials (<b>b</b>) on the immersion time of poly(2′,6′-dihydroxyacetophenone) in 10 mM acetonitrile solution of tributylamine containing 20 mM TBAP.</p>
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<p>Chronoamperometric curves of glassy carbon and platinum electrodes modified with poly(2′,6′-dihydroxyacetophenone) after washing with acetone with response to stirring at 700 rpm in 5 mM solution of hydroquinone with pH set to 7 with 0.05 mol/L phosphate buffer.</p>
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<p>Amperometric curve for hydroquinone during stirring at 700 rpm by sequential addition of stock solution for concentrations 0, 100, 200, 300, 400, and 500 mM with a poly(2′,6′-dihydroxyacetophenone)-modified platinum electrode (supporting electrolyte 0.05 M pH = 7 phosphate buffer, constant potential 0.5 V).</p>
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14 pages, 2150 KiB  
Article
Solvent-Focused Gas Chromatographic Determination of Thymol and Carvacrol Using Ultrasound-Assisted Dispersive Liquid–Liquid Microextraction through Solidifying Floating Organic Droplets (USA-DLLME-SFO)
by Sedigheh Barzegar, Mousab Rehmani, Mahdi Farahmandzadeh, Ghodratollah Absalan and Benson Karimi
Molecules 2024, 29(16), 3931; https://doi.org/10.3390/molecules29163931 - 20 Aug 2024
Viewed by 574
Abstract
An ultrasound-assisted dispersive liquid–liquid microextraction by solidifying floating organic droplets, coupled to a form of temperature-programmed gas chromatography flame ionization detection, has been developed for the extraction and determination of thymol and carvacrol. This method utilizes undecanol as the extraction solvent, offering advantages [...] Read more.
An ultrasound-assisted dispersive liquid–liquid microextraction by solidifying floating organic droplets, coupled to a form of temperature-programmed gas chromatography flame ionization detection, has been developed for the extraction and determination of thymol and carvacrol. This method utilizes undecanol as the extraction solvent, offering advantages such as facilitating phase transfer through solidification and enhancing solvent-focusing efficiency. The optimal gas chromatography conditions include a sample injection volume of 0.2 µL, a split ratio of 1:10, and a flow rate of 0.7 mL min−1. The extraction conditions entail an extraction solvent volume of 20 µL, a disperser solvent (acetone) volume of 500 µL, pH 7.0, 7.0% NaCl (3.5 M), a sample volume of 5.0 mL, an ultrasound duration of 10 min, and a centrifuge time of 7.5 min (800 rpm). These conditions enable the achievement of a high and reasonable linear range of 3.5 to 70. 0 μg mL−1 for both thymol and carvacrol. The detection limits are found to be 0.95 and 0.89 μg mL−1, respectively, for thymol and carvacrol. The obtained relative standard deviations, 2.7% for thymol and 2.6% for carvacrol, demonstrate acceptable precision for the purpose of quantitative analysis. Full article
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<p>Effect of extraction solvent. (<b>A</b>) Effect of the1-undecanol volume on the analytical signal in the determination of thymol (5.0 mg L<sup>−1</sup>) and carvacrol (5.0 mg L<sup>−1</sup>). Experimental conditions: disperser solvent (acetone) = 0.50 mL; (NaOH 1.0 M) pH 7.0; % NaCl = 7.0%; sample volume = 5.0 mL; ultrasound duration time = 10.0 min; centrifugation duration time (800 rpm) = 7.5 min (n = 3). (<b>B</b>) Effect of the dilution of the analytes on the optimization of the extraction solvent (1-undecanol) volume in the determination of thymol and carvacrol.</p>
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<p>Effect of the type of disperser solvent on the analytical signal under experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; disperser volume = 0.5 mL; pH 7.0; % NaCl = 7.0%; sample volume = 5.0 mL; ultrasound duration time = 10.0 min; and centrifuging duration time (at 800 rpm) = 7.5 min. (n = 3). (<b>A</b>) Determination of thymol (5.0 mg L<sup>−1</sup>). (<b>B</b>) Determination of carvacrol (5.0 mg L<sup>−1</sup>).</p>
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<p>Effect of the disperser solvent (acetone) volume on the analytical signal in the determination of thymol (5.0 mg L<sup>−1</sup>) and carvacrol (5.0 mg L<sup>−1</sup>). Experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; pH 7.0; % NaCl = 7.0%; sample volume = 5.0 mL; ultrasound duration time = 10.0 min; and centrifuging duration time (at 800 rpm) = 7.5 min (n = 3).</p>
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<p>Effect of the pH on the analytical signal in the determination of thymol (5.0 mg L<sup>−1</sup>) and carvacrol (5.0 mg L<sup>−1</sup>). Experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; disperser solvent (acetone) = 0.50 mL; % NaCl = 7.0%; sample volume = 5.0 mL; ultrasound duration time = 10.0 min; and centrifuging duration time (at 800 rpm) = 7.5 min (n = 3).</p>
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<p>Effect of the type of buffer solution on the analytical signal in the determination of thymol (5.0 mg L<sup>−1</sup>) and carvacrol (5.0 mg L<sup>−1</sup>). Experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; disperser solvent (acetone) = 0.50 mL; pH 7.0; % NaCl = 7.0%; sample volume = 5.0 mL; ultrasound duration time = 10.0 min; and centrifuging duration time (at 800 rpm) = 7.5 min.</p>
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<p>Effect of the % NaCl on the analytical signal in the determination of thymol (5.0 mg L<sup>−1</sup>) and carvacrol (5.0 mg L<sup>−1</sup>). Experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; disperser solvent (acetone) = 0.50 mL; pH 7.0; sample volume = 5.0 mL; ultrasound duration time = 10.0 min; and centrifuging duration time (at 800 rpm) = 7.5 min (n = 3).</p>
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<p>Effect of the sample volume on the analytical signal of thymol (5.0 mg L<sup>−1</sup>) and carvacrol (5.0 mg L<sup>−1</sup>). Experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; disperser solvent (acetone) = 0.50 mL; pH 7.0; %NaCl = 7.0%; ultrasound duration time = 10.0 min; and centrifuging duration time (at 800 rpm) = 7.5 min (n = 3).</p>
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<p>Calibration curve under experimental conditions: extractant solvent (1-undecanol) = 20.0 µL; disperser solvent (acetone) = 0.50 mL; pH 7.0; %NaCl = 7.0%; ultrasound duration time = 10.0 min; and centrifuging duration time = 7.5 min. (I/I<sub>IS</sub> = relative signal intensity of analyte to signal intensity of internal standard and C<sub>T</sub> = thymol concentration, C<sub>C</sub> = carvacrol concentration). (<b>A</b>) Thymol. (<b>B</b>) Carvacrol.</p>
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<p>Chromatograph for the determination of thymol and carvacrol. Conditions: extractant solvent: 1-undecanol (20.0 µL); disperser solvent = acetone (0.50 mL); pH 7.0; %NaCl = 7.0%; ultrasound duration time = 10.0 min; centrifuging duration time = 7.5 min.</p>
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13 pages, 2705 KiB  
Article
Development of a Neural Network for Target Gas Detection in Interdigitated Electrode Sensor-Based E-Nose Systems
by Kadir Kaya and Mehmet Ali Ebeoğlu
Sensors 2024, 24(16), 5315; https://doi.org/10.3390/s24165315 - 16 Aug 2024
Viewed by 738
Abstract
In this study, a neural network was developed for the detection of acetone, ethanol, chloroform, and air pollutant NO2 gases using an Interdigitated Electrode (IDE) sensor-based e-nose system. A bioimpedance spectroscopy (BIS)-based interface circuit was used to measure sensor responses in the [...] Read more.
In this study, a neural network was developed for the detection of acetone, ethanol, chloroform, and air pollutant NO2 gases using an Interdigitated Electrode (IDE) sensor-based e-nose system. A bioimpedance spectroscopy (BIS)-based interface circuit was used to measure sensor responses in the e-nose system. The sensor was fed with a sinusoidal voltage at 10 MHz frequency and 0.707 V amplitude. Sensor responses were sampled at 100 Hz frequency and converted to digital data with 16-bit resolution. The highest change in impedance magnitude obtained in the e-nose system against chloroform gas was recorded as 24.86 Ω over a concentration range of 0–11,720 ppm. The highest gas detection sensitivity of the e-nose system was calculated as 0.7825 Ω/ppm against 6.7 ppm NO2 gas. Before training with the neural network, data were filtered from noise using Kalman filtering. Principal Component Analysis (PCA) was applied to the improved signal data for dimensionality reduction, separating them from noise and outliers with low variance and non-informative characteristics. The neural network model created is multi-layered and employs the backpropagation algorithm. The Xavier initialization method was used for determining the initial weights of neurons. The neural network successfully classified NO2 (6.7 ppm), acetone (1820 ppm), ethanol (1820 ppm), and chloroform (1465 ppm) gases with a test accuracy of 87.16%. The neural network achieved this test accuracy in a training time of 239.54 milliseconds. As sensor sensitivity increases, the detection capability of the neural network also improves. Full article
(This article belongs to the Special Issue Chemical Sensors for Toxic Chemical Detection)
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<p>Block diagram for target gas detection.</p>
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<p>Experiment scheme for IDE sensor-based e-nose system.</p>
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<p>The view of the e-nose sensor system and the sensor array.</p>
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<p>The designed BPNN architecture.</p>
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<p>Flow diagram of the BPNN algorithm.</p>
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<p>The response of sensor-4 to chloroform gas.</p>
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<p>Sensors exhibit the highest impedance change response to acetone, ethanol, and chloroform gases.</p>
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<p>Sensor-2’s impedance change response to NO<sub>2</sub> gas in the concentration range of 0–46.7 ppm.</p>
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<p>MSE change graph of NO<sub>2</sub>–acetone–ethanol–chloroform gas classification with 87.16% test accuracy.</p>
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13 pages, 4401 KiB  
Article
Characterization of Nile Red-Stained Microplastics through Fluorescence Spectroscopy
by Suparnamaaya Prasad, Andrew Bennett and Michael Triantafyllou
J. Mar. Sci. Eng. 2024, 12(8), 1403; https://doi.org/10.3390/jmse12081403 - 15 Aug 2024
Viewed by 1726
Abstract
Microplastics (MPs), typically defined as plastic fragments smaller than 5 mm, are pervasive in terrestrial and marine ecosystems. There is a need for rapid, portable, low-cost detection systems to assess health and environmental risks. Fluorescent tagging with Nile Red (NR) has emerged as [...] Read more.
Microplastics (MPs), typically defined as plastic fragments smaller than 5 mm, are pervasive in terrestrial and marine ecosystems. There is a need for rapid, portable, low-cost detection systems to assess health and environmental risks. Fluorescent tagging with Nile Red (NR) has emerged as a popular detection method, but variations in fluorescent emissions based on NR solvent, plastic polymer, excitation wavelength, and additives complicate standardization. In this study, seven plastic samples stained with acetone-based NR were analyzed using a fluorescent spectrometer to identify optimal emission peaks across UV-Vis excitation wavelengths. These findings aid in selecting appropriate excitation wavelengths and optical filters for future detection systems. Additionally, a straightforward polymer identification scheme was validated against field-collected plastic samples, whose material composition was confirmed via Fourier Transform Infrared Spectroscopy. This work contributes towards developing accessible microplastic detection technologies by characterizing the fluorescent properties of NR-stained plastics and enhancing the capability for effective environmental monitoring. Future research will expand the dataset to include diverse plastics with varying additives and weathering, and incorporate computer-vision tools for automated data processing and polymer identification. Full article
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<p>Fluorescence spectroscopy experimental setup.</p>
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<p>Fluorescent emission spectra of Nile Red-stained lab plastics for different excitation wavelengths. Column (<b>left</b>) displays the spectra of plastics excited by 405 nm, plotted in blue on the left. Column (<b>middle</b>) displays the spectra of plastics excited by 465 nm, plotted in orange in the middle. Column (<b>right</b>) displays the spectra of plastics excited by 525 nm, plotted in yellow on the right [<a href="#B26-jmse-12-01403" class="html-bibr">26</a>].</p>
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<p>Polymer identification scheme [<a href="#B26-jmse-12-01403" class="html-bibr">26</a>].</p>
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<p>Fluorescent emission spectra of Nile Red-stained field plastics for different excitation wavelengths. Column on the left displays the spectra of PP plastics and column on the right displays the spectra of PE plastics [<a href="#B26-jmse-12-01403" class="html-bibr">26</a>].</p>
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<p>Low-cost microplastic imaging setup [<a href="#B26-jmse-12-01403" class="html-bibr">26</a>].</p>
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<p>Images of Nile Red-stained lab plastics for different excitation wavelengths [<a href="#B26-jmse-12-01403" class="html-bibr">26</a>]. Due to Nile Red’s solvatochromatic properties, the emission wavelength changes based on polarity of polymer surface.</p>
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<p>Images of Nile Red-stained lab plastics paired with raw fluorescent emission data for different excitation wavelengths [<a href="#B26-jmse-12-01403" class="html-bibr">26</a>].</p>
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15 pages, 7966 KiB  
Article
Anticandidal Properties of Launaea sarmentosa among the Salt Marsh Plants Collected from Palk Bay and the Gulf of Mannar Coast, Southeastern India
by Smriti Das, Karuppannagounder Rajan Priyanka, Kolandhasamy Prabhu, Ramachandran Vinayagam, Rajendran Rajaram and Sang Gu Kang
Antibiotics 2024, 13(8), 748; https://doi.org/10.3390/antibiotics13080748 - 9 Aug 2024
Viewed by 980
Abstract
Tidal wetlands, commonly known as salt marshes, are highly productive ecosystems in temperate regions worldwide. These environments constitute a unique flora composed primarily of salt-tolerant herbs, grasses, and shrubs. This study investigated the therapeutic properties of ten salt marsh plants collected mainly from [...] Read more.
Tidal wetlands, commonly known as salt marshes, are highly productive ecosystems in temperate regions worldwide. These environments constitute a unique flora composed primarily of salt-tolerant herbs, grasses, and shrubs. This study investigated the therapeutic properties of ten salt marsh plants collected mainly from Palk Bay and Mannar Gulf against Candida disease. This study examined the changes in natural plant products associated with their anti-Candida growth activity during two distinct seasonal changes—monsoon and summer. The potential of the salt marshes to inhibit the growth of five different Candida strains was assessed using four solvents. In phytochemical analysis, the extracts obtained from a Launaea sarmentosa exhibited the highest results compared to the other plant extracts. Fourier transform infrared spectroscopy revealed 12 peaks with alkane, aldehyde, amine, aromatic ester, phenol, secondary alcohol, and 1,2,3,4-tetrasubstituted. Gas-chromatography–mass spectrometry detected 30 compounds. Cyclotetracosane, lupeol, β-amyrin, and 12-oleanen-3-yl acetate showed the highest peak range. In particular, plant samples collected during the monsoon season were more effective in preventing Canda growth than the summer plant samples. In the monsoon season, the salt marsh plant extracted with ethyl acetate showed a high anti-Candida growth activity, while in the summer, the acetone extract exhibited a higher anti-Candida growth activity than the other solvents. The hexane extract of L. sarmentosa showed the highest inhibition zone against all Candidal strains. Furthermore, compounds, such as β-amyrin, lupeol, and oxirane, from the hexane extract of L. sarmentosa play a vital role in anti-Candida activity. This paper reports the potential of tidal marsh plant extracts for developing new antifungal agents for Candida infections. Full article
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<p>Anticandial properties of salt marsh plants exhibited as the zone of inhibition against Candidal strains during the monsoon season ((<b>a</b>)—Acetone; (<b>b</b>)—Ethyl Acetate; (<b>c</b>)—Methonal and (<b>d</b>)—Hexane).</p>
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<p>Anticandidal properties of salt marsh plants exhibiting zone of inhibition against Candidal strains during the summer season ((<b>a</b>)—Acetone; (<b>b</b>)—Ethyl acetate; (<b>c</b>)—Methanol; and (<b>d</b>)—Hexane).</p>
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<p>Anticandidal activity of saltmarsh plant <span class="html-italic">Launaea sarmentosa</span> extract exhibits the highest inhibition (CA—<span class="html-italic">Candida albicans</span>; CR—<span class="html-italic">Candida kefyr</span>; CKr—<span class="html-italic">Candida krusei;</span> CT—<span class="html-italic">Candida tropicalis</span>; CP—<span class="html-italic">Candida parapsilosis</span>).</p>
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<p>FT−IR spectrum showing the peaks obtained from the hexane extract of salt marsh <span class="html-italic">Launaea sarmentosa</span>.</p>
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<p>GC-MS showing the peaks obtained from the hexane extract of saltmarsh <span class="html-italic">Launaea sarmentosa</span>.</p>
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<p>Sampling sites of salt marsh plants collected from Palk Bay and the Gulf of Mannar.</p>
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<p>Salt marsh plants collected from Palk Bay and the Gulf of Mannar ((<b>A</b>) <span class="html-italic">Ipomoea pes-caprae</span>, (<b>B</b>) <span class="html-italic">Suaeda maritima</span>, (<b>C</b>) <span class="html-italic">Sesuvium portulacastrum</span>, (<b>D</b>) <span class="html-italic">Heliotropium curassavicum</span>, (<b>E</b>) <span class="html-italic">Launaea sarmentosa</span>, (<b>F</b>) <span class="html-italic">Bulbostylis barbata</span>, (<b>G</b>) <span class="html-italic">Salicornia brachiata</span>, (<b>H</b>) <span class="html-italic">Spinifex littoreus</span>, (<b>I</b>) Fim<span class="html-italic">bristylis spathacea</span>, and (<b>J</b>) <span class="html-italic">Artiplex halimus</span>).</p>
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22 pages, 4112 KiB  
Article
Impact of Processing on the Phenolic Content and Antioxidant Activity of Sorghum bicolor L. Moench
by Aduba Collins, Abishek Santhakumar, Sajid Latif, Kenneth Chinkwo, Nidhish Francis and Christopher Blanchard
Molecules 2024, 29(15), 3626; https://doi.org/10.3390/molecules29153626 - 31 Jul 2024
Cited by 2 | Viewed by 1069
Abstract
Sorghum, a cereal grain rich in nutrients, is a major source of phenolic compounds that can be altered by different processes, thereby modulating their phenolic content and antioxidant properties. Previous studies have characterised phenolic compounds from pigmented and non-pigmented varieties. However, the impact [...] Read more.
Sorghum, a cereal grain rich in nutrients, is a major source of phenolic compounds that can be altered by different processes, thereby modulating their phenolic content and antioxidant properties. Previous studies have characterised phenolic compounds from pigmented and non-pigmented varieties. However, the impact of processing via the cooking and fermentation of these varieties remains unknown. Wholegrain flour samples of Liberty (WhiteLi1 and WhiteLi2), Bazley (RedBa1 and RedBa2), Buster (RedBu1 and RedBu2), Shawaya black (BlackSb), and Shawaya short black 1 (BlackSs) were cooked, fermented, or both then extracted using acidified acetone. The polyphenol profiles were analysed using a UHPLC-Online ABTS and QTOF LC-MS system. The results demonstrated that combining the fermentation and cooking of the BlackSs and BlackSb varieties led to a significant increase (p < 0.05) in total phenolic content (TPC) and antioxidant activities, as determined through DPPH, FRAP, and ABTS assays. The 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical scavenging activity of WhiteLi1, BlackSb, RedBu2, and BlackSs increased by 46%, 32%, 25%, and 10%, respectively, post fermentation and cooking. Conversely, fermentation only or cooking generally resulted in lower phenolic content and antioxidant levels than when samples were fully processed compared to raw. Notably, most of the detected antioxidant peaks (53 phenolic compounds) were only detected in fermented and cooked black and red pericarp varieties. The phenolic compounds with the highest antioxidant activities in pigmented sorghum included 3-aminobenzoic acid, 4-acetylburtyic acid, malic acid, caffeic acid, and luteolin derivative. Furthermore, the growing location of Bellata, NSW, showed more detectable phenolic compounds following processing compared to Croppa Creek, NSW. This study demonstrates that sorghum processing releases previously inaccessible polyphenols, making them available for human consumption and potentially providing added health-promoting properties. Full article
(This article belongs to the Special Issue Natural Antioxidants in Functional Food)
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<p>Standard calibration curves for the determination of (<b>A</b>) total phenolic content and (<b>B</b>) total proanthocyanidin content (TPAC).</p>
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<p>UHPLC—Online ABTS overlaid changes in phenolic compounds after processing from black pericarp sorghum variety Shawaya short black 1 (BlackSs). * Compound detected in multiple processes. The numbers represent compounds identified in each process for BlackSs.</p>
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<p>UHPLC—Online ABTS overlaid changes in phenolic compounds after processing from red pericarp sorghum variety Buster (RedBu<sub>1</sub>). * Compound detected in multiple processes. The numbers represent compounds identified in each process for RedBu<sub>1</sub>.</p>
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<p>UHPLC—Online ABTS overlaid changes in phenolic compounds after processing from white pericarp sorghum variety Liberty (WhiteLi<sub>1</sub>). * Compound detected in multiple processes. The numbers represent compounds identified in each process for WhiteLi<sub>1</sub>.</p>
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<p>Variations in the phenolic composition (determined by a gallic acid standard curve in a UHPLC—Online ABTS system) of the significant phenolic compounds identified before and after processing of sorghum samples. Data are expressed as mg 100<sup>−1</sup> GAE and presented as mean ± SD; <span class="html-italic">n</span> = 3. Two—way ANOVA with multiple comparisons was performed, and statistical significance was set at <span class="html-italic">p</span> ≤ 0.05. * Statistically significant difference within processed sorghum samples. BlackSs, Shawaya short black 1; BlackSb, Shawaya black; RedBa<sub>1</sub> and RedBa<sub>2</sub>, Bazley; RedBu<sub>1</sub> and RedBu<sub>2</sub>, Buster; WhiteLi1 and WhiteLi2, Liberty; R, raw; C, cooked, F, fermented; FC, fermented and cooked.</p>
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<p>Changes to the ABTS antioxidant activity (determined by a Trolox standard curve in a UHPLC—Online ABTS system) of the significant phenolic compounds identified before and after processing of sorghum samples. Data are expressed as mg 100<sup>−1</sup> TE and presented as mean ± SD; <span class="html-italic">n</span> = 3. Two—way ANOVA with multiple comparisons was performed, and statistical significance was set at <span class="html-italic">p</span> ≤ 0.05. * Statistically significant difference within processed sorghum samples. BlackSs, Shawaya short black 1; BlackSb, Shawaya black; RedBa<sub>1</sub> and RedBa<sub>2</sub>, Bazley; RedBu<sub>1</sub> and RedBu<sub>2</sub>, Buster; WhiteLi<sub>1</sub> and WhiteLi<sub>2</sub>, Liberty; R, raw; C, cooked, F, fermented; FC, fermented and cooked.</p>
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