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Keywords = ultra high-pressure liquid chromatography quadrupole time-of-flight spectrometry (UHPLC/QTOF)

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20 pages, 1323 KiB  
Article
Screening of Pharmaceuticals in Surface Waters from Vhembe District, Limpopo Province, South Africa
by Uwineza Marie Clémentine Nibamureke and Irene Ellen Jane Barnhoorn
Water 2025, 17(3), 379; https://doi.org/10.3390/w17030379 - 30 Jan 2025
Cited by 1 | Viewed by 1486
Abstract
Pharmaceutical pollution of surface waters has emerged as a significant environmental health concern worldwide. In this study, we investigated the presence and concentration of pharmaceuticals in aquatic environments within Vhembe District Municipality, South Africa. To achieve this, grab samples of water were collected [...] Read more.
Pharmaceutical pollution of surface waters has emerged as a significant environmental health concern worldwide. In this study, we investigated the presence and concentration of pharmaceuticals in aquatic environments within Vhembe District Municipality, South Africa. To achieve this, grab samples of water were collected from various locations across the Thulamela Local Municipality encompassing rivers, streams, and dams. A targeted solid-phase extraction method with ultra-high-pressure liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS/MS) was used to screen, detect, and quantify 98 pharmaceutical compounds and caffeine in the collected water samples. The findings revealed the presence of a range of pharmaceutical compounds, including the antiretrovirals nevirapine and lopinavir, the anticonvulsant/antiepileptic carbamazepine, and the analgesic and antipyretic acetaminophen. The central nervous system stimulant caffeine was also detected in various water bodies across the region. The presence and concentrations of the pharmaceuticals varied across different water bodies, with nevirapine present at nine sites out of twenty-one (up to 166 ng/L), lopinavir at two sites (up to 42 ng/L), carbamazepine at one site (21 ng/L), and acetaminophen at two sites with the highest concentration of 427 ng/L. Caffeine was present at 15 sites (up to 975 ng/L). This study provides valuable insights into pharmaceutical pollution in surface water resources from one of South Africa’s rural areas, Vhembe District Municipality. It contributes to the monitoring data required to find sustainable solutions to the problem of pollutants of emerging concern in aquatic environments worldwide. Full article
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18 pages, 2563 KiB  
Article
In Vivo Metabolic Analysis of the Anticancer Effects of Plasma-Activated Saline in Three Tumor Animal Models
by Miao Qi, Dehui Xu, Shuai Wang, Bing Li, Sansan Peng, Qiaosong Li, Hao Zhang, Runze Fan, Hailan Chen and Michael G. Kong
Biomedicines 2022, 10(3), 528; https://doi.org/10.3390/biomedicines10030528 - 23 Feb 2022
Cited by 16 | Viewed by 2958
Abstract
In recent years, the emerging technology of cold atmospheric pressure plasma (CAP) has grown rapidly along with the many medical applications of cold plasma (e.g., cancer, skin disease, tissue repair, etc.). Plasma-activated liquids (e.g., culture media, water, or normal saline, previously exposed to [...] Read more.
In recent years, the emerging technology of cold atmospheric pressure plasma (CAP) has grown rapidly along with the many medical applications of cold plasma (e.g., cancer, skin disease, tissue repair, etc.). Plasma-activated liquids (e.g., culture media, water, or normal saline, previously exposed to plasma) are being studied as cancer treatments, and due to their advantages, many researchers prefer plasma-activated liquids as an alternative to CAP in the treatment of cancer. In this study, we showed that plasma-activated-saline (PAS) treatment significantly inhibited tumor growth, as compared with saline, in melanoma, and a low-pH environment had little effect on tumor growth in vivo. In addition, based on an ultra-high-performance liquid tandem chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) analysis of tumor cell metabolism, the glycerophospholipid metabolic pathway was the most susceptible metabolic pathway to PAS treatment in melanoma in vitro and in vivo. Furthermore, PAS also inhibited cell proliferation in vivo in oral tongue squamous-cell cancer and non-small-cell lung cancer. There were few toxic side effects in the three animal models, and the treatment was deemed safe to use. In the future, plasma-activated liquids may serve as a potential therapeutic approach in the treatment of cancer. Full article
(This article belongs to the Special Issue The Advances of Cold Plasma in the Biomedicines)
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20 pages, 2714 KiB  
Article
Assessment of Exposure to Di-(2-ethylhexyl) Phthalate (DEHP) Metabolites and Bisphenol A (BPA) and Its Importance for the Prevention of Cardiometabolic Diseases
by Fabrizia Carli, Demetrio Ciociaro and Amalia Gastaldelli
Metabolites 2022, 12(2), 167; https://doi.org/10.3390/metabo12020167 - 10 Feb 2022
Cited by 16 | Viewed by 5028
Abstract
Exposomics analyses have highlighted the importance of biomonitoring of human exposure to pollutants, even non-persistent, for the prevention of non-communicable diseases such as obesity, diabetes, non-alcoholic fatty liver disease, atherosclerosis, and cardiovascular diseases. Phthalates and bisphenol A (BPA) are endocrine disrupting chemicals (EDCs) [...] Read more.
Exposomics analyses have highlighted the importance of biomonitoring of human exposure to pollutants, even non-persistent, for the prevention of non-communicable diseases such as obesity, diabetes, non-alcoholic fatty liver disease, atherosclerosis, and cardiovascular diseases. Phthalates and bisphenol A (BPA) are endocrine disrupting chemicals (EDCs) widely used in industry and in a large range of daily life products that increase the risk of endocrine and cardiometabolic diseases especially if the exposure starts during childhood. Thus, biomonitoring of exposure to these compounds is important not only in adulthood but also in childhood. This was the goal of the LIFE-PERSUADED project that measured the exposure to phthalates (DEHP metabolites, MEHP, MEHHP, MEOHP) and BPA in Italian mother–children couples of different ages. In this paper we describe the method that was set up for the LIFE PERSUADED project and validated during the proficiency test (ICI/EQUAS) showing that accurate determination of urinary phthalates and BPA can be achieved starting from small sample size (0.5 mL) using two MS techniques applied in cascade on the same deconjugated matrix. Full article
(This article belongs to the Section Endocrinology and Clinical Metabolic Research)
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19 pages, 2896 KiB  
Article
Extraction Kinetics of Total Polyphenols, Flavonoids, and Condensed Tannins of Lentil Seed Coat: Comparison of Solvent and Extraction Methods
by Fernanda Galgano, Roberta Tolve, Teresa Scarpa, Marisa Carmela Caruso, Luigi Lucini, Biancamaria Senizza and Nicola Condelli
Foods 2021, 10(8), 1810; https://doi.org/10.3390/foods10081810 - 5 Aug 2021
Cited by 40 | Viewed by 4621
Abstract
The lentil seed coat is a waste by-product still rich in phenolic compounds, specifically condensed tannins. The effect of different solvents, as well as different processes, namely conventional solid–liquid extraction (CSLE) and ultrasound-assisted extraction (UAE), on the extraction yield of specific phenolic compound [...] Read more.
The lentil seed coat is a waste by-product still rich in phenolic compounds, specifically condensed tannins. The effect of different solvents, as well as different processes, namely conventional solid–liquid extraction (CSLE) and ultrasound-assisted extraction (UAE), on the extraction yield of specific phenolic compound classes was studied. Four empirical two-parameter models were examined to select the one that better fit the experimental data obtained under different operating conditions. Additionally, ultra-high-pressure liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPLC-ESI/QTOF-MS) was employed to profile the phenolic compounds obtained under distinct extraction conditions. In the operative conditions adopted here, the bioactive compounds yield achieved using UAE was lower than that obtained with CSLE. The kinetics of polyphenols, flavonoids, and condensed tannins extraction from the lentil seed coat were successfully fitted to the power-law models, yielding mean values of the root mean square < 5.4%, standard error of estimation < 0.53, and coefficient of determination > 0.8. In addition, the UHPLC-ESI/QTOF-MS of the lentil seed coat extracts allowed the putative recognition of nearly 500 compounds, mainly flavonoids and phenolic acids. Full article
(This article belongs to the Section Food Analytical Methods)
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15 pages, 4523 KiB  
Article
Biogenic ZnO Nanoparticles Synthesized Using a Novel Plant Extract: Application to Enhance Physiological and Biochemical Traits in Maize
by Daniele Del Buono, Alessandro Di Michele, Ferdinando Costantino, Marco Trevisan and Luigi Lucini
Nanomaterials 2021, 11(5), 1270; https://doi.org/10.3390/nano11051270 - 12 May 2021
Cited by 80 | Viewed by 5289
Abstract
The need to increase crop productivity and resistance directs interest in nanotechnology. Indeed, biogenic metal oxide nanoparticles can promote beneficial effects in plants, while their synthesis avoids the environmental impacts of conventional synthetic procedures. In this context, this research aimed to synthesize biogenic [...] Read more.
The need to increase crop productivity and resistance directs interest in nanotechnology. Indeed, biogenic metal oxide nanoparticles can promote beneficial effects in plants, while their synthesis avoids the environmental impacts of conventional synthetic procedures. In this context, this research aimed to synthesize biogenic zinc oxide nanoparticles (ZnO-NPs) using, for the first time, an extract of a wild and spontaneous aquatic species, Lemna minor (duckweed). The effectiveness of this biogenic synthesis was evidenced for comparison with non-biogenic ZnO-NPs (obtained without using the plant extract), which have been synthesized in this research. XRD (X-ray diffraction), FE-SEM (field emission gun electron scanning microscopy), EDX (energy dispersive x-ray spectroscopy), TEM (transmission electron microscope) and UV-vis (ultraviolet-visible spectrophotometry) showed the biogenic approach effectiveness. The duckweed extract was subjected to UHPLC-ESI/QTOF-MS (ultra high-pressure liquid chromatography quadrupole time of flight mass spectrometry) phenolic profiling. This untargeted characterization highlighted a high and chemically diverse content in the duckweed extract of compounds potentially implicated in nanoparticulation. From an application standpoint, the effect of biogenic nanoparticles was investigated on some traits of maize subjected to seed priming with a wide range of biogenic ZnO-NPs concentrations. Inductive effects on the shoot and root biomass development were ascertained concerning the applied dosage. Furthermore, the biogenic ZnO-NPs stimulated the content of chlorophylls, carotenoids, and anthocyanin. Finally, the study of malondialdehyde content (MDA) as a marker of the oxidative status further highlighted the beneficial and positive action of the biogenic ZnO-NPs on maize. Full article
(This article belongs to the Special Issue Green Biosynthesis of Nanostructures and Their Applications)
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30 pages, 2997 KiB  
Article
HPLC-DAD and UHPLC/QTOF-MS Analysis of Polyphenols in Extracts of the African Species Combretum padoides, C. zeyheri and C. psidioides Related to Their Antimycobacterial Activity
by Pia Fyhrquist, Enass Y. A. Salih, Satu Helenius, Into Laakso and Riitta Julkunen-Tiitto
Antibiotics 2020, 9(8), 459; https://doi.org/10.3390/antibiotics9080459 - 29 Jul 2020
Cited by 14 | Viewed by 4558
Abstract
Combretum padoides Engl. & Diels, C. psidioides Welv. and C. zeyheri Sond. are used for the treatment of infections and tuberculosis related symptoms in African traditional medicine. In order to verify these uses, extracts were screened for their growth inhibitory effects against M. [...] Read more.
Combretum padoides Engl. & Diels, C. psidioides Welv. and C. zeyheri Sond. are used for the treatment of infections and tuberculosis related symptoms in African traditional medicine. In order to verify these uses, extracts were screened for their growth inhibitory effects against M. smegmatis ATCC 14468. Ultra-high pressure liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UHPLC/QTOF-MS) and GC-MS were used to investigate the polyphenolic composition in the active extracts. The lowest minimum inhibitory concentration (MIC), 625 µg/mL, was shown by a methanol extract of the stem bark of C. psidioides. A butanol extract of C. psidioides gave large inhibition zone diameters (IZD 21 mm) and inhibited 84% of the mycobacterial growth at 312 µg/mL. Combretastatin B-2 and dihydrostilbene derivatives were present in the methanol extract of C. psidioides, whereas the butanol extract of this species contained punicalagin, corilagin, and sanguiin H-4. Methanol and butanol extracts of the stem bark of C. padoides gave large inhibition zone diameters (IZD 26.5 mm) and MIC values of 1250 and 2500 µg/mL, respectively. C. padoides contained an ellagitannin with a mass identical to punicalagin ([M-H] 1083.0587) and a corilagin like derivative ([M-H] 633.0750) as well as ellagic acid arabinoside and methyl ellagic acid xyloside. A butanol extract of the roots of C. zeyheri showed mild antimycobacterial activity and contained a gallotannin at m/z [M-H] 647.0894 as the main compound along with punicalagin and three unknown ellagitannins at m/z [M-H] 763.0788, 765.0566, and 817.4212. Our results indicate that the studied species of Combretum contain phenolic and polyphenolic compounds with possible potential as leads for antimycobacterial drugs or as adjuvants for conventional anti-TB drugs. Full article
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15 pages, 1556 KiB  
Article
Metabolomic Study to Evaluate the Transformations of Extra-Virgin Olive Oil’s Antioxidant Phytochemicals during In Vitro Gastrointestinal Digestion
by Gabriele Rocchetti, Biancamaria Senizza, Gianluca Giuberti, Domenico Montesano, Marco Trevisan and Luigi Lucini
Antioxidants 2020, 9(4), 302; https://doi.org/10.3390/antiox9040302 - 6 Apr 2020
Cited by 24 | Viewed by 4343
Abstract
In this work, different commercial extra-virgin olive oils (EVOO) were subjected to in vitro gastrointestinal digestion and the changes in bioactive compounds were evaluated by ultra-high-pressure liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry, using untargeted metabolomics. As expected, raw EVOO samples were abundant [...] Read more.
In this work, different commercial extra-virgin olive oils (EVOO) were subjected to in vitro gastrointestinal digestion and the changes in bioactive compounds were evaluated by ultra-high-pressure liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry, using untargeted metabolomics. As expected, raw EVOO samples were abundant in total sterols (on average: 3007.4 mg equivalents/kg) and tyrosol equivalents (on average: 334.1 mg equivalents/kg). However, the UHPLC-QTOF screening allowed us to annotate 309 compounds, with a large abundance of sterols (219 compounds), followed by polyphenols (67 compounds) and terpenoids. The in vitro gastrointestinal digestion was found to affect the phytochemical composition of the different EVOO samples. In particular, both unsupervised and supervised statistics depicted the modifications of the bioactive profile following gastric and pancreatic phases. Overall, the compounds which resulted as the most affected by the in vitro digestion were flavonoids (cyanidin and luteolin equivalents), whilst relatively high % bioaccessibility values were recorded for tyrosol equivalents during the pancreatic phase (on average, 66%). In this regard, oleuropein-aglycone (i.e., the major phenolic compound in EVOO) was converted to hydroxytyrosol, moving from an average value of 1.3 (prior to the in vitro digestion) up to 9.7 mg equivalents/kg during the pancreatic step. As proposed in the literature, the increase in hydroxytyrosol might be the result of the combined effect of lipase(s) activity and acidic conditions. Taken together, the present findings corroborate the suitability of untargeted metabolomics coupled to in vitro digestion methods to investigate the bioaccessibility of phenolic compounds. In this regard, a significant impact of in vitro gastrointestinal digestion on polyphenolic profiles has been detected, thus suggesting the need to account for actual bioaccessibility values rather than just considering the amounts in the raw commodity. Full article
(This article belongs to the Special Issue Olive Oil Antioxidants)
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20 pages, 1812 KiB  
Article
Untargeted Metabolomic Profiling, Multivariate Analysis and Biological Evaluation of the True Mangrove (Rhizophora mucronata Lam.)
by Nabeelah Bibi Sadeer, Gabriele Rocchetti, Biancamaria Senizza, Domenico Montesano, Gokhan Zengin, Ahmet Uysal, Rajesh Jeewon, Luigi Lucini and Mohamad Fawzi Mahomoodally
Antioxidants 2019, 8(10), 489; https://doi.org/10.3390/antiox8100489 - 16 Oct 2019
Cited by 32 | Viewed by 6395
Abstract
Currently, there is a renewed interest towards the development of plant-based pharmacophores. In this work, 16 extracts prepared from the leaves, twigs, roots and fruits of a hydro-halophyte, Rhizophora mucronata Lam. (Family: Rhizophoraceae), were studied for possible antioxidant activity and the phenolic profiles [...] Read more.
Currently, there is a renewed interest towards the development of plant-based pharmacophores. In this work, 16 extracts prepared from the leaves, twigs, roots and fruits of a hydro-halophyte, Rhizophora mucronata Lam. (Family: Rhizophoraceae), were studied for possible antioxidant activity and the phenolic profiles established. Thereafter, enzymatic inhibitory activities (α-amylase, α-glucosidase, tyrosinase, acetyl- (AChE), butyrylcholinesterase (BChE), lipase, and elastase) were assessed. The total phenolic, flavonoid, phenolic acid, tannin, flavanol and triterpenoid content were estimated using standard assays. An untargeted metabolomics-based approach, based on ultra-high-pressure liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry (UHPLC-QTOF-MS) followed by multivariate statistics, was then used to comprehensively profile and describe the phenolics present. UHPLC-QTOF-MS allowed for putatively annotating 104 phenolic acids, 103 flavonols, 94 flavones, 71 anthocyanins, 66 tyrosols, 29 lignans, 15 alkylphenols and 10 stilbenes in the extracts. Nine strains (Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumoniae, Methicillin-resistant Staphylococcus aureus (MRSA), Salmonella enteritidis, Sarcina lutea, Proteus mirabilis, Bacillus cereus and Candida albicans) were then used to investigate the antimicrobial properties. The methanolic twig extract exhibited significant reducing potential towards Cu (II)/Cu (I) and Fe (III)/Fe (II) (1336.88 ± 15.70 and 710.18 ± 21.04 mg TE/g, respectively) and was the most potent DPPH radical scavenger (807.07 ± 6.83 mg TE/g). Additionally, the methanolic twig extract showed significant inhibition against most targeted enzymes. Anti-microbial results showed that all extracts were active against MRSA. Multivariate analysis demonstrated that the phenolic profile of ethyl acetate extracts and leaves were the two most discriminative parameters in terms of solvents and organs, respectively. The present findings indicated that R. mucronata may be further explored for the management/prevention of oxidative stress, neurodegenerative complications and hyperpigmentation. Full article
(This article belongs to the Special Issue Phenolic Profiling and Antioxidant Capacity in Plants)
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17 pages, 3063 KiB  
Article
Metabolic Profiling of Pyrrolizidine Alkaloids in Foliage of Two Echium spp. Invaders in Australia—A Case of Novel Weapons?
by Dominik Skoneczny, Paul A. Weston, Xiaocheng Zhu, Geoff M. Gurr, Ragan M. Callaway and Leslie A. Weston
Int. J. Mol. Sci. 2015, 16(11), 26721-26737; https://doi.org/10.3390/ijms161125979 - 6 Nov 2015
Cited by 32 | Viewed by 8406
Abstract
Metabolic profiling allows for simultaneous and rapid annotation of biochemically similar organismal metabolites. An effective platform for profiling of toxic pyrrolizidine alkaloids (PAs) and their N-oxides (PANOs) was developed using ultra high pressure liquid chromatography quadrupole time-of-flight (UHPLC-QTOF) mass spectrometry. Field-collected populations of [...] Read more.
Metabolic profiling allows for simultaneous and rapid annotation of biochemically similar organismal metabolites. An effective platform for profiling of toxic pyrrolizidine alkaloids (PAs) and their N-oxides (PANOs) was developed using ultra high pressure liquid chromatography quadrupole time-of-flight (UHPLC-QTOF) mass spectrometry. Field-collected populations of invasive Australian weeds, Echium plantagineum and E. vulgare were raised under controlled glasshouse conditions and surveyed for the presence of related PAs and PANOs in leaf tissues at various growth stages. Echium plantagineum possessed numerous related and abundant PANOs (>17) by seven days following seed germination, and these were also observed in rosette and flowering growth stages. In contrast, the less invasive E. vulgare accumulated significantly lower levels of most PANOs under identical glasshouse conditions. Several previously unreported PAs were also found at trace levels. Field-grown populations of both species were also evaluated for PA production and highly toxic echimidine N-oxide was amongst the most abundant PANOs in foliage of both species. PAs in field and glasshouse plants were more abundant in the more widely invasive species, E. plantagineum, and may provide competitive advantage by increasing the plant’s capacity to deter natural enemies in its invaded range through production of novel weapons. Full article
(This article belongs to the Special Issue Metabolomics in the Plant Sciences)
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