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1
Scendoni, Roberto, Emanuele Bury, Erika Buratti, Rino Froldi, Marta Cippitelli, Gianmario Mietti, and Mariano Cingolani. "Detection of Morphine and Opioids in Fingernails: Immunohistochemical Analysis and Confirmation with Ultra-High-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry." Toxics 10, no. 8 (July 26, 2022): 420. http://dx.doi.org/10.3390/toxics10080420.
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This study aimed to investigate the detection of morphine in fingernails from forensic autopsies using immunohistochemistry (IHC), with confirmation by ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS). A primary antibody specific to morphine and a secondary antibody conjugated to horseradish peroxidase (HRP) was used. IHC on specimens of Subjects A and B (both drug addicts) resulted in the detection of morphine on a cell layer of the nail plate matrix. UHPLC-HRMS and GC-MS analysis showed that Subject A had a morphine concentration of 0.35 ng/mg in the fingernail and 472 ng/mL in the blood, while Subject B reached 1.23 ng/mg in the fingernail and 360 ng/ml in the blood. Most of those matrices were positive for codeine, methadone, EDDP, and 6-MAM. The use of IHC in Subject C (a former addict) showed no positivity for morphine in the fingernail, while the UHPLC-HRMS analysis confirmed its absence in the fingernail and blood. Additionally, an analysis of the scalp or pubic hair of the subjects was carried out using UHPLC-HRMS. The results suggest that IHC can be used to establish the site of accumulation of morphine in the nail matrix; for postmortem diagnosis; and that basic substances can be detected by UHPLC-HRMS. There are no previous studies on the use of IHC as a technique for forensic purposes in unconventional matrices, such as nails.
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Cao, Shanshan, Min Hu, Lingli Yang, Meiqin Li, Zhen Shi, Wenming Cheng, Yazhong Zhang, Fei Chen, Sheng Wang, and Qunlin Zhang. "Chemical Constituent Analysis of Ranunculus Sceleratus L. Using Ultra-High-Performance Liquid Chromatography Coupled with Quadrupole-Orbitrap High-Resolution Mass Spectrometry." Molecules 27, no. 10 (May 20, 2022): 3299. http://dx.doi.org/10.3390/molecules27103299.
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Ranunculus sceleratus L.(RS) has shown various pharmacological effects in traditional Chinese medicine. In our previous study, the positive therapeutic effect on α-naphthylisothiocyanate induced intrahepatic cholestasis in rats was obtained using TianJiu treatment with fresh RS. However, the chemical profile of RS has not been clearly clarified, which impedes the research progress on the therapeutic effect of RS. Herein, an ultra-high performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) method was developed to rapidly separate and identify multiple constituents in the 80% methanol extract of RS. A total of sixty-nine compounds (19 flavonoids, 22 organic acids, 6 coumarins, 4 lignans, 14 nitrogenous compounds, and 4 anthraquinones) were successfully characterized. A total of 12 of these compounds were unambiguously identified by standard samples. Their mass spectrometric fragmentation pathways were investigated. It is worth noting that flavonoids and lignans were identified for the first time in RS. In this study, we successfully provide the first comprehensive report on identifying major chemical constituents in RS by UHPLC-Q-Orbitrap HRMS. The obtained results enrich the RS chemical profile, paving the way for further phytochemical study, quality control, and pharmacological investigation of RS.
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Tao, Ye, Yannick Rossez, Clovis Bortolus, Luminita Duma, Faustine Dubar, and Franck Merlier. "Simultaneous Quantification of Trehalose and Trehalose 6-Phosphate by Hydrophilic Interaction Chromatography/Electrospray Accurate Mass Spectrometry with Application in Non-Targeted Metabolomics." Molecules 28, no. 8 (April 13, 2023): 3443. http://dx.doi.org/10.3390/molecules28083443.
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High-resolution mass spectrometry (HRMS) was coupled with ultra-high-performance liquid chromatography (UHPLC) to simultaneously quantify trehalose and trehalose 6-phosphate without derivatization or sample preparation. The use of full scan mode and exact mass analysis also makes it possible to carry out metabolomic analyses as well as semi-quantification. In addition, the use of different clusters in negative mode makes it possible to compensate for deficiencies in linearity and inerrant saturation at time-of-flight detectors. The method has been approved and validated for different matrices, yeasts, and bacteria, and has shown differentiation between bacteria as a function of growth temperatures.
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Filatova, Daria, Oscar Núñez, and Marinella Farré. "Ultra-Trace Analysis of Cyanotoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry." Toxins 12, no. 4 (April 11, 2020): 247. http://dx.doi.org/10.3390/toxins12040247.
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The increasing frequency of episodes of harmful algal blooms of cyanobacterial origin is a risk to ecosystems and human health. The main human hazard may arise from drinking water supply and recreational water use. For this reason, efficient multiclass analytical methods are needed to assess the level of cyanotoxins in water reservoirs and tackle these problems. This work describes the development of a fast, sensitive, and robust analytical method for multiclass cyanotoxins determination based on dual solid-phase extraction (SPE) procedure using a polymeric cartridge, Oasis HLB (Waters Corporation, Milford, MA, USA), and a graphitized non-porous carbon cartridge, SupelcleanTM ENVI-CarbTM (Sigma-Aldrich, St. Louis, MO, USA), followed by ultra-high-performance liquid chromatography high-resolution mass spectrometry (SPE-UHPLC-HRMS). This method enabled the analysis of cylindrospermopsin, anatoxin-a, nodularin, and seven microcystins (MC-LR, MC-RR, MC-YR, MC-LA, MC-LY, MC-LW, MC-LF). The method limits of detection (MLOD) of the validated approach were between 4 and 150 pg/L. The analytical method was applied to assess the presence of the selected toxins in 21 samples collected in three natural water reservoirs in the Ter River in Catalonia (NE of Spain) used to produce drinking water for Barcelona city (Spain).
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Cui, Zhifeng, Zhe Li, Weichao Dong, Lili Qiu, Jiayu Zhang, and Shaoping Wang. "Comprehensive Metabolite Identification of Genipin in Rats Using Ultra-High-Performance Liquid Chromatography Coupled with High Resolution Mass Spectrometry." Molecules 28, no. 17 (August 29, 2023): 6307. http://dx.doi.org/10.3390/molecules28176307.
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Genipin, an aglycone of geniposide, is a rich iridoid component in the fruit of Gardenia jasminoides Ellis and has numerous biological activities. However, its metabolic profiles in vivo and vitro remain unclear. In this study, an effective analytical strategy based on ultra-high-performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) in positive and negative ion modes was developed to analyze and identify genipin metabolites in rat urine, blood, feces, and fecal fermentation in combination with many methods including post-collection data mining methods, high-resolution extracted ion chromatography (HREIC), and multiple mass defect filtering (MMDF). Simultaneously, the metabolites of genipin in vivo were verified by fecal fermentation of SD rats at different times. Finally, based on information such as reference substances, chromatographic retention behavior, and accurate mass determination, a total of 50 metabolites (including prototypes) were identified in vivo. Among them, 7, 31 and 28 metabolites in vivo were identified in blood, urine, and feces, respectively. Our results showed that genipin could generate different metabolites that underwent multiple metabolic reactions in vivo including methylation, hydroxylation, dehydroxylation, hydrogenation, sulfonation, glucuronidation, demethylation, and their superimposed reactions. Forty-six metabolites were verified in vitro. Meanwhile, 2 and 19 metabolites identified in blood and urine were also verified in fecal fermentation at different times. These results demonstrated that metabolites were produced in feces and reabsorbed into the body. In conclusion, the newly discovered metabolites of genipin can provide a new perspective for understanding its pharmacological effects and build the foundation for thee toxicity and safety evaluations of genipin.
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Agostini, Marco, Donata Favretto, Caterina Renzoni, Susanna Vogliardi, and Andrea Duranti. "Characterization of URB Series Synthetic Cannabinoids by HRMS and UHPLC–MS/MS." Pharmaceuticals 16, no. 2 (January 29, 2023): 201. http://dx.doi.org/10.3390/ph16020201.
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A large number of synthetic cannabinoids are included in new psychoactive substances (NPS) and constitute an open research area in analytical pharmaceutical and toxicology when methods are needed to unambiguously identify these substances and their metabolites in biological fluids. A full molecular characterization of five synthetic molecules of the URB series that is able to interact with the endocannabinoid system was achieved with a high-resolution mass spectrometry (HRMS) in positive ion electrospray ionization and collisional experiments on the protonated parent ions, obtaining characteristic fragmentation patterns. Ultra-high-performance liquid chromatography coupled with a triple quadrupole (UHPLC-MS/MS) has also been used, which can help develop methods for screening and confirming synthetic cannabinoids in biological fluids.
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Pezzatti, Julian, Víctor González-Ruiz, Julien Boccard, Davy Guillarme, and Serge Rudaz. "Evaluation of Different Tandem MS Acquisition Modes to Support Metabolite Annotation in Human Plasma Using Ultra High-Performance Liquid Chromatography High-Resolution Mass Spectrometry for Untargeted Metabolomics." Metabolites 10, no. 11 (November 15, 2020): 464. http://dx.doi.org/10.3390/metabo10110464.
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Ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS) is a powerful and essential technique for metabolite annotation in untargeted metabolomic applications. The aim of this study was to evaluate the performance of diverse tandem MS (MS/MS) acquisition modes, i.e., all ion fragmentation (AIF) and data-dependent analysis (DDA), with and without ion mobility spectrometry (IM), to annotate metabolites in human plasma. The influence of the LC separation was also evaluated by comparing the performance of MS/MS acquisition in combination with three complementary chromatographic separation modes: reversed-phase chromatography (RPLC) and hydrophilic interaction chromatography (HILIC) with either an amide (aHILIC) or a zwitterionic (zHILIC) stationary phase. RPLC conditions were first chosen to investigate all the tandem MS modes, and we found out that DDA did not provide a significant additional amount of chemical coverage and that cleaner MS/MS spectra can be obtained by performing AIF acquisitions in combination with IM. Finally, we were able to annotate 338 unique metabolites and demonstrated that zHILIC was a powerful complementary approach to both the RPLC and aHILIC chromatographic modes. Moreover, a better analytical throughput was reached for an almost negligible loss of metabolite coverage when IM-AIF and AIF using ramped instead of fixed collision energies were used.
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El-Hawary, Enas A., Ahmed Zayed, Annegret Laub, Luzia V. Modolo, Ludger Wessjohann, and Mohamed A. Farag. "How Does LC/MS Compare to UV in Coffee Authentication and Determination of Antioxidant Effects? Brazilian and Middle Eastern Coffee as Case Studies." Antioxidants 11, no. 1 (January 7, 2022): 131. http://dx.doi.org/10.3390/antiox11010131.
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Coffee is a popular beverage owing to its unique flavor and diverse health benefits. The current study aimed at investigating the antioxidant activity, in relation to the phytochemical composition, of authenticated Brazilian green and roasted Coffea arabica and C. robusta, along with 15 commercial specimens collected from the Middle East. Ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-ESI–HRMS) and UV spectrometry were employed for profiling and fingerprinting, respectively. With the aid of global natural product social molecular networking (GNPS), a total of 88 peaks were annotated as belonging to different chemical classes, of which 11 metabolites are reported for the first time in coffee seeds. Moreover, chemometric tools showed comparable results between both platforms, with more advantages for UV in the annotation of roasting products, suggesting that UV can serve as a discriminative tool. Additionally, antioxidant assays coupled with the UHPLC-ESI–HRMS dataset using partial least-squares discriminant analysis (PLS-DA) demonstrated that caffeoylquinic acid and caffeine were potential antioxidant markers in unroasted coffee versus dicaffeoyl quinolactone and melanoidins in roasted coffee. The study presents a multiplex metabolomics approach to the quality control of coffee, one of the most consumed beverages.
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Nuzzo, Genoveffa, Emiliano Manzo, Marcello Ziaco, Laura Fioretto, Ana Margarida Campos, Carmela Gallo, Giuliana d’Ippolito, and Angelo Fontana. "UHPLC-MS Method for the Analysis of the Molecular Adjuvant Sulfavant A." Applied Sciences 11, no. 4 (February 5, 2021): 1451. http://dx.doi.org/10.3390/app11041451.
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A fast and sensitive method that is based on Ultra High Performance Liquid Chromatography coupled with High Resolution Mass Spectrometry (UHPLC-HRMS) for the measurement of Sulfavant A, a molecular adjuvant with a sulfolipid skeleton, is described. The method has been validated over the linearity range of 2.5–2000 ngmL−1 using a deuterated derivative (d70-Sulfavant A) as internal standard. Chromatographic separation is based on a UHPLC Kinetex® 2.6 µm PS C18 column and a gradient of methanol in 0.32 mM ammonium hydroxide solution buffered at pH 8. The lowest limit of quantification of Sulfavant A was 6.5 ngmL−1. The analytical procedure was tested on an extract of mice lung spiked with 30, 300, and 1500 ng of Sulfavant A. The analysis revealed a precision and accuracy value (as a mean value of all the quality control samples analyzed) of 4.7% and 96% in MeOH and 6.4% and 93.4% in the lung extracts, respectively.
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Hong, Junting, Nadia Boussetta, Gérald Enderlin, Nabil Grimi, and Franck Merlier. "Real-Time Monitoring of the Atrazine Degradation by Liquid Chromatography and High-Resolution Mass Spectrometry: Effect of Fenton Process and Ultrasound Treatment." Molecules 27, no. 24 (December 17, 2022): 9021. http://dx.doi.org/10.3390/molecules27249021.
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High resolution mass spectrometry (HRMS) was coupled with ultra-high-performance liquid chromatography (uHPLC) to monitor atrazine (ATZ) degradation process of Fenton/ultrasound (US) treatment in real time. Samples were automatically taken through a peristaltic pump, and then analysed by HPLC-HRMS. The injection in the mass spectrometer was performed every 4 min for 2 h. ATZ and its degradation metabolites were sampled and identified. Online Fenton experiments in different equivalents of Fenton reagents, online US experiments with/without Fe2+ and offline Fenton experiments were conducted. Higher equivalents of Fenton reagents promoted the degradation rate of ATZ and the generation of the late-products such as Ammeline (AM). Besides, adding Fe2+ accelerated ATZ degradation in US treatment. In offline Fenton, the degradation rate of ATZ was higher than that of online Fenton, suggesting the offline samples were still reacting in the vial. The online analysis precisely controls the effect of reagents over time through automatic sampling and rapid detection, which greatly improves the measurement accuracy. The experimental set up proposed here both prevents the degradation of potentially unstable metabolites and provides a good way to track each metabolite.
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Tsagkaris, Aristeidis S., Nela Prusova, Zbynek Dzuman, Jana Pulkrabova, and Jana Hajslova. "Regulated and Non-Regulated Mycotoxin Detection in Cereal Matrices Using an Ultra-High-Performance Liquid Chromatography High-Resolution Mass Spectrometry (UHPLC-HRMS) Method." Toxins 13, no. 11 (November 5, 2021): 783. http://dx.doi.org/10.3390/toxins13110783.
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Cereals represent a widely consumed food commodity that might be contaminated by mycotoxins, resulting not only in potential consumer health risks upon dietary exposure but also significant financial losses due to contaminated batch disposal. Thus, continuous improvement of the performance characteristics of methods to enable an effective monitoring of such contaminants in food supply is highly needed. In this study, an ultra-high-performance liquid chromatography coupled to a hybrid quadrupole orbitrap mass analyzer (UHPLC-q-Orbitrap MS) method was optimized and validated in wheat, maize and rye flour matrices. Nineteen analytes were monitored, including both regulated mycotoxins, e.g., ochratoxin A (OTA) or deoxynivalenol (DON), and non-regulated mycotoxins, such as ergot alkaloids (EAs), which are analytes that are expected to be regulated soon in the EU. Low limits of quantification (LOQ) at the part per trillion level were achieved as well as wide linear ranges (four orders of magnitude) and recovery rates within the 68–104% range. Overall, the developed method attained fit-for-purpose results and it highlights the applicability of high-resolution mass spectrometry (HRMS) detection in mycotoxin food analysis.
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Lima da Silva, Juliane, Sonia Lombardi, Luigi Castaldo, Elena Morelli, Jaqueline Garda-Buffon, Luana Izzo, and Alberto Ritieni. "Multi-Mycotoxin Analysis in Italian Grains Using Ultra-High-Performance Chromatography Coupled to Quadrupole Orbitrap Mass Spectrometry." Toxins 15, no. 9 (September 8, 2023): 562. http://dx.doi.org/10.3390/toxins15090562.
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Mycotoxins are a major source of contamination in cereals, posing risks to human health and causing significant economic losses to the industry. A comprehensive strategy for the analysis of 21 mycotoxins in Italian cereal grain samples (n = 200) was developed using a simple and quick sample preparation method combined with ultra-high-performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry (UHPLC Q-Orbitrap HRMS). The proposed method showed some advantages, such as multi-mycotoxin analyses with simple sample preparation, fast determination, and high sensitivity. The analysis of the sample revealed the presence of 11 mycotoxins, with α-zearalenol being the most frequently detected, while deoxynivalenol exhibited the highest contamination level. Furthermore, co-occurrence was identified in 15.5% of the samples under analysis. Among these, 13% of the samples reported the simultaneous presence of two mycotoxins, while 2.5% showed the co-occurrence of three mycotoxins. Currently, there has been a renewed interest in guaranteeing the quality and safety of products intended for human consumption. This study holds significant value due to its ability to simultaneously detect multiple mycotoxins within a complex matrix. Furthermore, it provides findings regarding the occurrence and co-occurrence of emerging mycotoxins that currently lack regulation under the existing European Commission Regulation.
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Revelou, Panagiota-Kyriaki, Maroula G. Kokotou, and Violetta Constantinou-Kokotou. "Identification of Auxin Metabolites in Brassicaceae by Ultra-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry." Molecules 24, no. 14 (July 18, 2019): 2615. http://dx.doi.org/10.3390/molecules24142615.
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Auxins are signaling molecules involved in multiple stages of plant growth and development. The levels of the most important auxin, indole-3-acetic acid (IAA), are regulated by the formation of amide and ester conjugates with amino acids and sugars. In this work, IAA and IAA amide conjugates with amino acids bearing a free carboxylic group or a methyl ester group, along with some selected IAA metabolites, were studied in positive and negative electrospray ionization (ESI) modes, utilizing high-resolution mass spectrometry (HRMS) as a tool for their structural analysis. HRMS/MS spectra revealed the fragmentation patterns that enable us to identify IAA metabolites in plant extracts from eight vegetables of the Brassicaceae family using a fast and reliable ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QToF-MS) method. The accurate m/z (mass to charge) ratio and abundance of the molecular and fragment ions of the studied compounds in plant extracts matched those obtained from commercially available or synthesized compounds and confirmed the presence of IAA metabolites.
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Sah, Samyukta, Sylvia R. Yun, David A. Gaul, Andro Botros, Eun Young Park, Olga Kim, Jaeyeon Kim, and Facundo M. Fernández. "Targeted Microchip Capillary Electrophoresis-Orbitrap Mass Spectrometry Metabolomics to Monitor Ovarian Cancer Progression." Metabolites 12, no. 6 (June 9, 2022): 532. http://dx.doi.org/10.3390/metabo12060532.
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The lack of effective screening strategies for high-grade serous carcinoma (HGSC), a subtype of ovarian cancer (OC) responsible for 70–80% of OC related deaths, emphasizes the need for new diagnostic markers and a better understanding of disease pathogenesis. Capillary electrophoresis (CE) coupled with high-resolution mass spectrometry (HRMS) offers high selectivity and sensitivity for ionic compounds, thereby enhancing biomarker discovery. Recent advances in CE-MS include small, chip-based CE systems coupled with nanoelectrospray ionization (nanoESI) to provide rapid, high-resolution analysis of biological specimens. Here, we describe the development of a targeted microchip (µ) CE-HRMS method, with an acquisition time of only 3 min and sample injection volume of 4nL, to analyze 40 target metabolites in serum samples from a triple-mutant (TKO) mouse model of HGSC. Extracted ion electropherograms showed sharp, baseline resolved peak shapes, even for structural isomers such as leucine and isoleucine. All calibration curves of the analytes maintained good linearity with an average R2 of 0.994, while detection limits were in the nM range. Thirty metabolites were detected in mouse serum with recoveries ranging from 78 to 120%, indicating minimal ionization suppression and good accuracy. We applied the µCE-HRMS method to biweekly-collected serum samples from TKO and TKO control mice. A time-resolved analysis revealed characteristic temporal trends for amino acids, nucleosides, and amino acid derivatives. These metabolic alterations are indicative of altered nucleotide biosynthesis and amino acid metabolism in HGSC development and progression. A comparison of the µCE-HRMS dataset with non-targeted ultra-high performance liquid chromatography (UHPLC)–MS results showed identical temporal trends for the five metabolites detected with both platforms, indicating the µCE-HRMS method performed satisfactorily in terms of capturing metabolic reprogramming due to HGSC progression while reducing the total data collection time three-fold.
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Li, Baohong, Yingjie Fu, Hui Xi, Shan Liu, Wuduo Zhao, Peng Li, Wu Fan, Dingzhong Wang, and Shihao Sun. "Untargeted Metabolomics Using UHPLC-HRMS Reveals Metabolic Changes of Fresh-Cut Potato during Browning Process." Molecules 28, no. 8 (April 11, 2023): 3375. http://dx.doi.org/10.3390/molecules28083375.
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Surface browning plays a major role in the quality loss of fresh-cut potatoes. Untargeted metabolomics were used to understand the metabolic changes of fresh-cut potato during the browning process. Their metabolites were profiled by ultra-high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS). Data processing and metabolite annotation were completed by Compound Discoverer 3.3 software. Statistical analysis was applied to screen the key metabolites correlating with browning process. Fifteen key metabolites responsible for the browning process were putatively identified. Moreover, after analysis of the metabolic causes of glutamic acid, linolenic acid, glutathione, adenine, 12-OPDA and AMP, we found that the browning process of fresh-cut potatoes was related to the structural dissociation of the membrane, oxidation and reduction reaction and energy shortage. This work provides a reference for further investigation into the mechanism of browning in fresh-cut products.
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Rocchetti, Gabriele, Francesca Ghilardelli, Francesco Masoero, and Antonio Gallo. "Screening of Regulated and Emerging Mycotoxins in Bulk Milk Samples by High-Resolution Mass Spectrometry." Foods 10, no. 9 (August 28, 2021): 2025. http://dx.doi.org/10.3390/foods10092025.
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In this work, a retrospective screening based on ultra-high-performance liquid chromatography (UHPLC) coupled with high-resolution mass spectrometry (HRMS) based on Orbitrap-Q-Exactive Focus™ was used to check the occurrence of regulated and emerging mycotoxins in bulk milk samples. Milk samples were collected from dairy farms in which corn silage was the main ingredient of the feeding system. The 45 bulk milk samples were previously analyzed for a detailed untargeted metabolomic profiling and classified into five clusters according to the corn silage contamination profile, namely: (1) low levels of Aspergillus- and Penicillium-mycotoxins; (2) low levels of fumonisins and other Fusarium-mycotoxins; (3) high levels of Aspergillus-mycotoxins; (4) high levels of non-regulated Fusarium-mycotoxins; (5) high levels of fumonisins and their metabolites. Multivariate statistics based on both unsupervised and supervised analyses were used to evaluate the significant fold-change variations of the main groups of mycotoxins detected when comparing milk samples from clusters 3, 4, and 5 (high contamination levels of the corn silages) with cluster 1 and 2 (low contamination levels of the corn silages). Overall, 14 compounds showed a significant prediction ability, with antibiotic Y (VIP score = 2.579), bikaverin (VIP score = 1.975) and fumonisin B2 (VIP score = 1.846) being the best markers. The k-means clustering combined with supervised statistics showed two discriminant groups of milk samples, thus revealing a hierarchically higher impact of the whole feeding system (rather than the only corn silages) together with other factors of variability on the final mycotoxin contamination profile. Among the discriminant metabolites we found some Fusarium mycotoxins, together with the tetrapeptide tentoxin (an Alternaria toxin), the α-zearalenol (a catabolite of zearalenone), mycophenolic acid and apicidin. These preliminary findings provide new insights into the potential role of UHPLC-HRMS to evaluate the contamination profile and the safety of raw milk to produce hard cheese.
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Bravi, Viviana S., Sandra Castello, and Luis Bruno-Blanch. "Phytochemical preliminary study of hexane fractions of leaves of Eugenia uniflora L. (Myrtaceae)." Boletin Latinoamericano y del Caribe de Plantas Medicinales y Aromaticas 22, no. 1 (January 30, 2023): 86–99. http://dx.doi.org/10.37360/blacpma.23.22.1.7.
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Fractions from the Hexane Extract (HE) of Eugenia unifloraL. leaves were subjected to various chromatographic systems. Germacrone sesquiterpene and bornyl acetate bicyclic ester were characterized by High Performance Liquid Chromatography coupled to Mass Spectrometry (HPLC-MS) with APCI Mass detector comparing with their homonymous spectrum provided by databases and characteristic fragmentation pathways were proposed. The monoterpene pulegone and the pentacyclic triterpene compound, ursolic acid, were found through High Performance Liquid Chromatography coupled to High Resolution Mass Spectrometry (HPLC -HRMS) by atmospheric pressure ionization (API) and the detector used was mass of Electronic Impact (IE). Both ursolic acid and bornyl acetate are present in other species of the same genus, but not in the species studied.
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Giang, Le Truong, and Tran Lam Thanh Thien. "Determination of aflatoxin B1, B2, G1, G2 in cashew nut by UHPLC‐HRMS." Vietnam Journal of Chemistry 58, no. 4 (August 2020): 540–47. http://dx.doi.org/10.1002/vjch.202000027.
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AbstractIn recent years, Vietnam is the leading country in exporting cashew to global market. However, tropical climate is a significantly favorable condition for fungus to develop when the cashew is not properly stored. For this reason, mycotoxin contaminations are likely to occur on the cashew, especially aflatoxin. By utilizing solid phase extraction technique with Oasis HLB stationary phase and optimizing conditions of sample preparation, the toxins such as aflatoxin B1, B2, G1 and G2 were extracted and concentrated from cashew samples. Simultaneously, with the assistance of ultra high‐performance liquid chromatography coupled with high resolution mass spectrometry detector, this study has successfully fabricated concurrent analysis method of aflatoxin compounds with high sensitivity and selectivity. The method established in this study manifested a high linear range (R2 ≥ 0.995), sensitivity (limits of detection ranged from 0.05 to 0.10 μg/kg and limits of quantification varied from 0.5 to 1.0 μg/kg), adequate recovery (96.5‐109.4 %), and good repeatability (intra‐day precision in the range of 2.2‐6.1 % and inter‐day precision in the range of 3.6‐13.3 %). In particular, this method has been successfully applied for the determination of 4 aflatoxins in real cashew nut samples.
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Tahri, Wiem, Abdelwaheb Chatti, Roberto Romero-González, Noelia López-Gutiérrez, Antonia Garrido Frenich, and Ahmed Landoulsi. "Phenolic profiling of the aerial part of Chrysanthemum trifurcatum using ultra high performance liquid chromatography coupled to Orbitrap high resolution mass spectrometry." Analytical Methods 8, no. 17 (2016): 3517–27. http://dx.doi.org/10.1039/c6ay00365f.
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Gheorghiu, Oana Ramona Cătălina, Anne Marie Ciobanu, Claudia Maria Guțu, Carmen Lidia Chițescu, Giorgiana Valentina Costea, Daniela Mădălina Anghel, Ana Maria Vlasceanu, and Daniela Luiza Baconi. "Determination of Phosphodiesterase Type-5 Inhibitors (PDE-5) in Dietary Supplements." Molecules 28, no. 10 (May 16, 2023): 4116. http://dx.doi.org/10.3390/molecules28104116.
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This study proposed a high-performance thin-layer chromatography (HPTLC) screening method to detect phosphodiesterase 5 (PDE-5) inhibitors as possible adulterant agents in various dietary supplements. Chromatographic analysis was performed on silica gel 60F254 plates using a mixture of ethyl acetate:toluene:methanol:ammonia in a volume ratio of 50:30:20:0.5 as a mobile phase. The system provided compact spots and symmetrical peaks of sildenafil and tadalafil with retardation factor values of 0.55 and 0.90, respectively. The analysis of products purchased from the internet or specialized stores demonstrated the presence of sildenafil, tadalafil, or both compounds in 73.3% of products, highlighting inadequacies and inconsistencies in the labeling, as all dietary supplements were declared to be natural. The results were confirmed using ultra-high-performance liquid chromatography coupled with a positive electrospray ionization high-resolution tandem mass spectrometry (UHPLC-HRMS-MS) method. Furthermore, in some samples, vardenafil and various analogs of PDE-5 inhibitors were detected using a non-target HRMS-MS approach. The results of the quantitative analysis revealed similar findings between the two methods, with adulterant quantities found to be similar to or higher than those in approved medicinal products. This study demonstrated that the HPTLC method is a suitable and economical method for screening PDE-5 inhibitors as adulterants in dietary supplements intended for sexual activity enhancement.
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Wang, Jian, Wendy Cheung, and Willis Chow. "Ultra-High Performance Liquid Chromatography/Electrospray Ionization-Tandem Mass Spectrometry Determination of 151 Pesticides in Soybeans and Pulses." Journal of AOAC INTERNATIONAL 96, no. 5 (September 1, 2013): 1114–33. http://dx.doi.org/10.5740/jaoacint.12-465.
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Abstract This paper presents the application of ultra-high performance LC (UHPLC) and MS for the determination of 151 pesticides in soybeans and pulses. A core-shell particle (2.6 μm particle size) column and a fully porous sub-2 μm (1.7 μm particle size) column showed comparable performance in chromatographic resolution and separation, increasing selectivity, and reducing analysis time. UHPLC was coupled with either a triple quadrupole mass analyzer (MS/MS) or a quadrupole Orbitrap (namely Orbital trap) mass spectrometer (Q-Orbitrap MS), which possesses fast data acquisition capability. Both configurations yielded analytical run times of ≤14 min. Soybean and pulse samples were analyzed and quantitated for pesticide residues using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure, UHPLC/electrospray ionization (ESI)-MS/MS, and matrix-matched standard calibration curves (in an analytical range of 5–500 μg/kg) with isotopically-labeled standards or a chemical analog as internal standards. The method performance parameters that included overall recovery, intermediate precision, and measurement uncertainty were evaluated according to a nested design experiment. Approximately 89% of the pesticides studied had recoveries between 81 and 110%; 95%, had intermediate precision ≤20%; and 93% showed measurement uncertainty ≤40%. From a pilot study of 100 samples, eight tested positive by UHPLC/ESI-MS/MS for carbendazim, methomyl, or imidacloprid. These pesticides were further confirmed using UHPLC/ESI-Q-Orbitrap MS based on accurate mass measurement with mass error ≤5 ppm.
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Narváez, Alfonso, Yelko Rodríguez-Carrasco, Luigi Castaldo, Luana Izzo, and Alberto Ritieni. "Ultra-High-Performance Liquid Chromatography Coupled with Quadrupole Orbitrap High-Resolution Mass Spectrometry for Multi-Residue Analysis of Mycotoxins and Pesticides in Botanical Nutraceuticals." Toxins 12, no. 2 (February 12, 2020): 114. http://dx.doi.org/10.3390/toxins12020114.
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Cannabidiol (CBD) food supplements made of Cannabis sativa L. extracts have quickly become popular products due to their health-promoting effects. However, potential contaminants, such as mycotoxins and pesticides, can be coextracted during the manufacturing process and placed into the final product. Accordingly, a novel methodology using ultra-high-performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was developed to quantify 16 mycotoxins produced by major C. sativa fungi, followed by a post-target screening of 283 pesticides based on a comprehensive spectral library. The validated procedure was applied to ten CBD-based products. Up to six different Fusarium mycotoxins were found in seven samples, the most prevalent being zearalenone (60%) and enniatin B1 (30%), both found at a maximum level of 11.6 ng/g. Co-occurrence was observed in four samples, including one with enniatin B1, enniatin A and enniatin A1. On the other hand, 46 different pesticides were detected after retrospective analysis. Ethoxyquin (50%), piperonyl butoxide (40%), simazine (30%) and cyanazine (30%) were the major residues found. These results highlight the necessity of monitoring contaminants in food supplements in order to ensure a safe consumption, even more considering the increase trend in their use. Furthermore, the developed procedure is proposed as a powerful analytical tool to evaluate the potential mycotoxin profile of these particular products.
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Formisano, Luigi, Michele Ciriello, Christophe El-Nakhel, Milena Poledica, Giuseppe Starace, Giulia Graziani, Alberto Ritieni, Stefania De Pascale, and Youssef Rouphael. "Pearl Grey Shading Net Boosts the Accumulation of Total Carotenoids and Phenolic Compounds That Accentuate the Antioxidant Activity of Processing Tomato." Antioxidants 10, no. 12 (December 15, 2021): 1999. http://dx.doi.org/10.3390/antiox10121999.
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Tomato (Solanum lycopersicum L.) is one of the most consumed vegetables worldwide due to its low caloric intake and high fiber, minerals, and phenolic compounds, making it a high-quality functional food. However, fruit quality attributes can be affected by pre-harvest factors, especially environmental stresses. This research aimed to evaluate the influence of two shading nets (white net −30% and pearl grey net −40% shading degree) on the yield and phytochemical profile of tomato fruits grown in summer under the Mediterranean climate. Mineral and organic acid content (by ion chromatography-IC), phenolic profile (by ultra-high performance liquid chromatography-UHPLC coupled with an Orbitrap high-resolution mass spectrometry-HRMS), carotenoid content (by high-performance liquid chromatography with diode array detection-HPLC-DAD), and antioxidant activities DPPH, ABTS, and FRAP (by UV-VIS spectrophotometry) were determined. Tomato fruits grown under the pearl grey net recorded the highest values of total phenolic compounds (14,997 µg 100 g−1 of fresh weight) and antioxidant activities DPPH, ABTS, and FRAP, without affecting either fruit color or marketable yield. The reduction of solar radiation through pearl grey nets proved to be an excellent tool to increase the phytochemical quality of tomato fruits during summer cultivation in a Mediterranean environment.
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Labsvards, Kriss Davids, Vita Rudovica, Rihards Kluga, Janis Rusko, Lauma Busa, Maris Bertins, Ineta Eglite, Jevgenija Naumenko, Marina Salajeva, and Arturs Viksna. "Determination of Floral Origin Markers of Latvian Honey by Using IRMS, UHPLC-HRMS, and 1H-NMR." Foods 11, no. 1 (December 24, 2021): 42. http://dx.doi.org/10.3390/foods11010042.
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The economic significance of honey production is crucial; therefore, modern and efficient methods of authentication are needed. During the last decade, various data processing methods and a combination of several instrumental methods have been increasingly used in food analysis. In this study, the chemical composition of monofloral buckwheat (Fagopyrum esculentum), clover (Trifolium repens), heather (Calluna vulgaris), linden (Tilia cordata), rapeseed (Brassica napus), willow (Salix cinerea), and polyfloral honey samples of Latvian origin were investigated using several instrumental analysis methods. The data from light stable isotope ratio mass spectrometry (IRMS), ultra-high performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS), and nuclear magnetic resonance (NMR) analysis methods were used in combination with multivariate analysis to characterize honey samples originating from Latvia. Results were processed using the principal component analysis (PCA) to study the potential possibilities of evaluating the differences between honey of different floral origins. The results indicate the possibility of strong differentiation of heather and buckwheat honeys, and minor differentiation of linden honey from polyfloral honey types. The main indicators include depleted δ15N values for heather honey protein, elevated concentration levels of rutin for buckwheat honey, and qualitative presence of specific biomarkers within NMR for linden honey.
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Schusterova, Dana, Jana Hajslova, Vladimir Kocourek, and Jana Pulkrabova. "Pesticide Residues and Their Metabolites in Grapes and Wines from Conventional and Organic Farming System." Foods 10, no. 2 (February 2, 2021): 307. http://dx.doi.org/10.3390/foods10020307.
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In this study, the occurrence of pesticide residues and their metabolites in grapes and wines was investigated. A targeted analysis of 406 pesticide residues in 49 wine and grape samples from organic and conventional production were performed using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction method, followed by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry. Multiple residues (>4 residues/sample) were detected in 22 tested samples. The most commonly detected residues were fungicides (e.g., boscalid) and insecticides (e.g., methoxyfenozide). An ultra-high-performance liquid chromatography–high resolution mass spectrometry method (UHPLC–(HR)MS) was used for screening of pesticide metabolites. We also provide a method and database for detecting pesticide metabolites (extending our previously published database to 49 metabolites originating from 25 pesticides). An introduced strategy of targeted screening of pesticide metabolites was applied for authentication of 27 organic grapes and wines. In total, 23 samples were free of quantifiable residues/detected metabolites or contained residues approved for organic production.
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Kang, Ye-Ji, Hyeon-Cheol Jeong, Tae-Eun Kim, and Kwang-Hee Shin. "Bioanalytical Method Using Ultra-High-Performance Liquid Chromatography Coupled with High-Resolution Mass Spectrometry (UHPL-CHRMS) for the Detection of Metformin in Human Plasma." Molecules 25, no. 20 (October 11, 2020): 4625. http://dx.doi.org/10.3390/molecules25204625.
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Metformin is the first-line medicine for the treatment of type 2 diabetes. Drug interactions between metformin and other drugs, food, or beverages cannot only cause changes in the pharmacokinetic profiles but also affect the efficacy of metformin. The purpose of this study was to develop a rapid and reliable bioanalytical method for the detection of plasma metformin concentration in humans. To remove interfering substances in plasma, acidified acetonitrile (acetonitrile containing 0.1% formic acid) was added to samples. Ultra-high-performance liquid chromatography (UHPLC) coupled with high resolution mass spectrometry (HRMS) was used to analyze metformin and its internal standard (metformin-d6). Analyte separation was performed on a BEH HILIC analytical column (100 × 2.1 mm, 1.7 μm) using a gradient elution of 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B). The total chromatographic run time was 2 min. The developed method was validated for its linearity, accuracy and precision, selectivity (signal of interfering substance; analyte, lower limit of quantification (LLOQ) ≤ 20%; IS, IS ≤ 5%), sensitivity (LLOQ, 5 ng/mL; S/N ratio ≥ 10), stability (low quality control (LQC, 15 ng/mL), 2.95–14.19%; high quality control (HQC, 1600 ng/mL), −9.49–15.10%), dilution integrity (diluted QC (4000 ng/mL); 10-folds diluted QC (400 ng/mL); 5-folds diluted QC (800 ng/mL); accuracy, 81.30–91.98%; precision, ≤4.47%), carry-over (signal of double blank; analyte, LLOQ ≤20%; IS, IS ≤5%), and matrix effect (LQC, 10.109%; HQC, 12.271%) under various conditions. The constructed calibration curves were shown linear in the concentration range of 5–2000 ng/mL, with within- and between-run precision values of <8.19% and accuracy in the range of 91.13–105.25%. The plasma metformin concentration of 16 healthy subjects was successfully measured by applying the validated bioanalytical method.
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Tareq, Fakir Shahidullah, Raghavendhar R. Kotha, Savithiry Natarajan, Jianghao Sun, and Devanand L. Luthria. "An Untargeted Metabolomics Approach to Study the Variation between Wild and Cultivated Soybeans." Molecules 28, no. 14 (July 19, 2023): 5507. http://dx.doi.org/10.3390/molecules28145507.
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The differential metabolite profiles of four wild and ten cultivated soybeans genotypes were explored using an untargeted metabolomics approach. Ground soybean seed samples were extracted with methanol and water, and metabolic features were obtained using ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS) in both positive and negative ion modes. The UHPLC-HRMS analysis of the two different extracts resulted in the putative identification of 98 metabolites belonging to several classes of phytochemicals, including isoflavones, organic acids, lipids, sugars, amino acids, saponins, and other compounds. The metabolic profile was significantly impacted by the polarity of the extraction solvent. Multivariate analysis showed a clear difference between wild and cultivated soybean cultivars. Unsupervised and supervised learning algorithms were applied to mine the generated data and to pinpoint metabolites differentiating wild and cultivated soybeans. The key identified metabolites differentiating wild and cultivated soybeans were isoflavonoids, free amino acids, and fatty acids. Catechin analogs, cynaroside, hydroxylated unsaturated fatty acid derivatives, amino acid, and uridine diphosphate-N-acetylglucosamine were upregulated in the methanol extract of wild soybeans. In contrast, isoflavonoids and other minor compounds were downregulated in the same soybean extract. This metabolic information will benefit breeders and biotechnology professionals to develop value-added soybeans with improved quality traits.
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D’Archivio, Angelo, Francesca Di Donato, Martina Foschi, Maria Maggi, and Fabrizio Ruggieri. "UHPLC Analysis of Saffron (Crocus sativus L.): Optimization of Separation Using Chemometrics and Detection of Minor Crocetin Esters." Molecules 23, no. 8 (July 25, 2018): 1851. http://dx.doi.org/10.3390/molecules23081851.
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Ultra-high performance liquid chromatography (UHPLC) coupled with diode array detection (DAD) was applied to improve separation and detection of mono- and bis-glucosyl esters of crocetin (crocins), the main red-colored constituents of saffron (Crocus sativus L.), and other polar components. Response surface methodology (RSM) was used to optimise the chromatographic resolution on the Kinetex C18 (Phenomenex) column taking into account of the combined effect of the column temperature, the eluent flow rate and the slope of a linear eluent concentration gradient. A three-level full-factorial design of experiments was adopted to identify suitable combinations of the above factors. The influence of the separation conditions on the resolutions of 22 adjacent peaks was simultaneously modelled by a multi-layer artificial neural network (ANN) in which a bit string representation was used to identify the target analytes. The chromatogram collected under the optimal separation conditions revealed a higher number of crocetin esters than those already characterised by means of mass-spectrometry data and usually detected by HPLC. Ultra-high performance liquid chromatography analyses carried out on the novel Luna Omega Polar C18 (Phenomenex) column confirmed the large number of crocetin derivatives. Further work is in progress to acquire mass-spectrometry data and to clarify the chemical structure to the newly found saffron components.
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Narváez, Alfonso, Luana Izzo, Noelia Pallarés, Luigi Castaldo, Yelko Rodríguez-Carrasco, and Alberto Ritieni. "Human Biomonitoring of T-2 Toxin, T-2 Toxin-3-Glucoside and Their Metabolites in Urine through High-Resolution Mass Spectrometry." Toxins 13, no. 12 (December 5, 2021): 869. http://dx.doi.org/10.3390/toxins13120869.
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The metabolic profile of T-2 toxin (T-2) and its modified form T-2-3-glucoside (T-2-3-Glc) remain unexplored in human samples. Therefore, the present study aimed to investigate the presence of T-2, T-2-3-Glc and their respective major metabolites in human urine samples (n = 300) collected in South Italy through an ultra-high performance liquid chromatography (UHPLC) coupled to Q-Orbitrap-HRMS methodology. T-2 was quantified in 21% of samples at a mean concentration of 1.34 ng/mg Crea (range: 0.22–6.54 ng/mg Crea). Almost all the major T-2 metabolites previously characterized in vitro were tentatively found, remarking the occurrence of 3′-OH-T-2 (99.7%), T-2 triol (56%) and HT-2 (30%). Regarding T-2-3-Glc, a low prevalence of the parent mycotoxin (1%) and its metabolites were observed, with HT-2-3-Glc (17%) being the most prevalent compound, although hydroxylated products were also detected. Attending to the large number of testing positive for T-2 or its metabolites, this study found a frequent exposure in Italian population.
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Reinholds, I., G. Juodeikiene, E. Bartkiene, D. Zadeike, V. Bartkevics, V. Krungleviciute, D. Cernauskas, and D. Cižeikiene. "Evaluation of ozonation as a method for mycotoxins degradation in malting wheat grains." World Mycotoxin Journal 9, no. 3 (June 1, 2016): 409–17. http://dx.doi.org/10.3920/wmj2015.2011.
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The influence of ozone (O3) gas on reducing the contamination with Fusarium mycotoxins in malting wheat grains was investigated. Ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS) and Orbitrap high resolution mass spectrometry (UHPLC-Orbitrap-HRMS) were used to determine mycotoxins in wheat grains before and 40 to 130 min after the exposure to 20 mg/l O3. Pearson’s analysis (R2=0.96-0.98) showed a good correlation between the performance efficiency of both mass spectrometry quantification techniques. The concentrations of determined mycotoxins (zearalenone (ZEA): 19.5-459 µg/kg, deoxynivalenol (DON): 3,370-4,620 µg/kg, T-2 toxin: 19.5-35.4 µg/kg, and HT-2 toxin: 258-819 µg/kg) decreased notably, depending on the duration of contact with ozone. A notable elimination of ZEA, HT-2, and T-2 in wheat grain was observed: the content of these compounds was reduced on average by 58.6, 64.6, and 62%, respectively, already after 40 min of ozonation. The effect was less pronounced in the case of DON, for which the average degradation rate reached the maximum of only 25% after 130 min exposure. We conclude that ozonation for up to 130 min was effective for reducing the content of most mycotoxins determined in this study, except for DON, in contaminated grains to concentrations below the acceptable maximum levels in wheat in accordance to the EU regulations.
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Syahfitr, Sari Anggraini, and Dan Ridho Asra. "Analysis of Medicinal Chemicals Contained on Jamu: A Review." Asian Journal of Pharmaceutical Research and Development 9, no. 2 (April 15, 2021): 33–46. http://dx.doi.org/10.22270/ajprd.v9i2.931.
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Background: Jamu is commonly known as an Indonesian traditional herbal medicine that contains ingredients or ingredients derived from plants, animals, minerals, galenic, or mixtures of these ingredients that have been hereditary for medicinal use. Some studies reported the presence of medicinal chemicals that are deliberately added to Jamu. Jamuthat containing medicinal chemicals usually had a faster healing effect compared to Jamu that do not contain medicinal chemicals. Jamu added medicinal chemicals cause serious side effects if it is consumed regularly, overdose, and long period consumption with uncontrolled dosage or its interaction with other substances on jamu formulation.
Purpose: This review article aims to summarize several methods used to analyze medicinal chemicals contained in jamu.
Data source:The author created thisreview article by conducting literature studies. The literature was collected from national and international journals published in the last ten years (2010-2020). The works of literature were collected from trusted online journal sites such as the digital library, Google, Google scholar/Google Cendekia, PubMed, ScienceDirect, NCBI, Researchgate, and other E-resource with the keyword “Jamu”, “medicinal chemicals”, and “analysis of medicinal chemicals”.
Conclusion: Jamu products that containing medicinal chemicals are jamu pegal linu, weight loss, stamina enhancer, diabetes, antihypertensive and dietary supplements. The medicinal chemicals used are sodium diclofenac, paracetamol, piroxicam, ibuprofen, dexamethasone, mefenamic acid, phenolphthalein, sibutramine, fenfluramine, sildenafil, tadalafil, thiosildenafil, caffeine, ephedrine, nifedipine, glibenclamide. Herbal Medicine was analyzed by the TLC method (thin layer chromatography), Densitometry-chromatography, thin-layer chromatography-Spectrophotometry, SERS-thin layer chromatography, Spectrophotometry, HPLC (High-Performance Liquid Chromatography), HPLC-ESI-MS/MS (high-performance liquid. chromatography/electrospray ionization tandem mass spectrometry), HPLC-Densitometry (High-Performance Liquid Chromatography-densitometry), UHPLC-Q-ORTIP HERMS (ultra-high-performance liquid chromatography-Quadrupole-orbitrap high-resolution mass spectrometry), UPLC/Q-TOF MS (ultra-performance liquid chromatography (UPLC) coupled with quadrupole-time-of-flight mass spectrometry (Q-TOF MS), Capillary electrophoresis (CE), GC-MS (Gas Chromatography-Mass Spectrometry), LC-MS (Liquid Crhomatogaph Mass) Spectrometry), Prototype Test-Strip, Infrared spectroscopy.
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Guan, Huanyu, Pengfei Li, Qian Wang, Fanli Zeng, Daoping Wang, Mei Zhou, Meng Zhou, Xun He, Shanggao Liao, and Weidong Pan. "Systematically Exploring the Chemical Ingredients and Absorbed Constituents of Polygonum capitatum in Hyperuricemia Rat Plasma Using UHPLC-Q-Orbitrap HRMS." Molecules 27, no. 11 (May 30, 2022): 3521. http://dx.doi.org/10.3390/molecules27113521.
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Polygonum capitatum as an ethnic medicine has been used to treat urinary tract infections, pyelonephritis and urinary calculi. In our previous study, P. capitatum was found to have anti-hyperuricemia effects. Nevertheless, the active constituents of P. capitatum for treating hyperuricemia were still unclear. In this study, an ultra-high-performance liquid chromatography coupled to quadrupole/orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was used to comprehensively detect the chemical ingredients of P. capitatum and its absorbed constituents in the plasma of hyperuricemia rats for the first time. Xcalibur 3.0 and Compound Discoverer 2.0 software coupled to mzCloud and ChemSpider databases were utilized for qualitative analysis. A total of 114 chemical components including phenolics, flavonoids, tannins, phenylpropanoids, amino acids, amides and others were identified or tentatively characterized based on the exact mass, retention time and structural information. Compared to the previous P. capitatum study, an additional 66 different components were detected. Moreover, 68 related xenobiotics including 16 prototype components and 52 metabolites were found in the plasma of hyperuricemia rats. The metabolic pathways included ring fission, hydrolysis, decarboxylation, dehydroxylation, methylation, glucuronidation and sulfation. This work may provide important information for further investigation on the active constituents of P. capitatum and their action mechanisms for anti-hyperuricemia effects.
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Sardari, Roya R. R., Jens Prothmann, Olavur Gregersen, Charlotta Turner, and Eva Nordberg Karlsson. "Identification of Phlorotannins in the Brown Algae, Saccharina latissima and Ascophyllum nodosum by Ultra-High-Performance Liquid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry." Molecules 26, no. 1 (December 23, 2020): 43. http://dx.doi.org/10.3390/molecules26010043.
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Phlorotannins are bioactive polyphenols in brown macroalgae that make these algae interesting as healthy food. Specific phlorotannins are, however, seldom identified, and extracts from different species are often only analysed for total phenolic content (TPC). In this study, our focus was to identify phlorotannin molecules from Saccharina latissima and Ascophyllum nodosum (a species rich in these compounds) using ultra-high-performance liquid chromatography coupled to high-resolution tandem mass spectrometry (UHPLC-HRMS2). Water and ethanol (30 and 80% v/v) were used at solid:liquid ratios, extraction times and temperatures, proposed to result in high TPC in extracts from other species. The S. latissima extracts, however, did not allow phlorotannin detection by either UHPLC-UV/Vis or UHPLC-HRMS2, despite a TPC response by the Folin–Ciocalteu assay, pinpointing a problem with interference by non-phenolic compounds. Purification by solid phase extraction (SPE) led to purer, more concentrated fractions and identification of four phlorotannin species in A. nodosum and one in S. latissima by UHPLC-HRMS2, using extracts in ethanol 80% v/v at a solid:liquid ratio of 1:10 for 20 h at 25 °C with an added 10 h at 65 °C incubation of remaining solids. The phlorotannin with the formula C12H10O7 (corresponding to bifuhalol) is the first identified in S. latissima.
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Romanet, Remy, Florian Bahut, Maria Nikolantonaki, and Régis D. Gougeon. "Molecular Characterization of White Wines Antioxidant Metabolome by Ultra High Performance Liquid Chromatography High-Resolution Mass Spectrometry." Antioxidants 9, no. 2 (January 28, 2020): 115. http://dx.doi.org/10.3390/antiox9020115.
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The knowledge about the molecular fraction contributing to white wines oxidative stability is still poorly understood. However, the role of S- and N-containing compounds, like glutathione and other peptides, as a source of reductant in many oxidation reactions, and acting against heavy metals toxicity, or lipid and polyphenol oxidation as ROS-scavenger is today very well established. In that respect, the aim of the present study is to introduce an original analytical tool for the direct determination of the available nucleophilic compounds in white wine under acidic pH conditions. One step derivatization of nucleophiles has been realized directly in wines using 4-methyl-1,2-benzoquinone (4MeQ) as an electrophilic probe. Derivatization conditions considering probe concentration, pH, reaction time, MS ionisation conditions and adducts stability, were optimized using model solutions containing standard sulfur and amino compounds (GSH, Cys, HCys and Ser-Aps-Cys-Asp-Ser, Asp-Met, Met and Glu). Ultra-high-performance liquid chromatography coupled to a quadrupole-time of flight mass spectrometer (UHPLC-QqTOF-MS) analysis of up to 92 white wines from different cultivars (Chardonnay, Sauvignon and Semillon) followed by Multivariate analysis (PLS DA) and Wilcoxon test allowed to isolate up to 141 putative wine relevant nucleophiles. Only 20 of these compounds, essentially thiols, were detectable in samples before derivatization, indicating the importance of the quinone trapping on the revelation of wine unknown nucleophiles. Moreover, annotation using online database (Oligonet, Metlin and KEGG) as well as elementary formula determined by isotopic profile, provided evidence of the presence of amino acids (Val, Leu, Ile, Pro, Trp, Cys and Met) and peptides with important antioxidant properties. The complimentary set of MS/MS spectral data greatly accelerated identification of nucleophiles and enabled peptides sequencing. These results show that probing wines with 4-methyl-1,2-benzoquinone enhances thiols ionisation capacity and gives a better screening of specific S- N- containing functional compounds as part of the white wines antioxidant metabolome.
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Wang, Jing, Jie Cui, Ziyi Liu, Yang Yang, Zhan Li, and Huiling Liu. "Untargeted Metabolomics Based on Ultra-High-Performance Liquid Chromatography Coupled with Quadrupole Orbitrap High-Resolution Mass Spectrometry for Differential Metabolite Analysis of Pinelliae Rhizoma and Its Adulterants." Molecules 29, no. 9 (May 6, 2024): 2155. http://dx.doi.org/10.3390/molecules29092155.
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The present study investigates the chemical composition variances among Pinelliae Rhizoma, a widely used Chinese herbal medicine, and its common adulterants including Typhonium flagelliforme, Arisaema erubescens, and Pinellia pedatisecta. Utilizing the non-targeted metabolomics technique of employing UHPLC-Q-Orbitrap HRMS, this research aims to comprehensively delineate the metabolic profiles of Pinelliae Rhizoma and its adulterants. Multivariate statistical methods including PCA and OPLS-DA are employed for the identification of differential metabolites. Volcano plot analysis is utilized to discern upregulated and downregulated compounds. KEGG pathway analysis is conducted to elucidate the differences in metabolic pathways associated with these compounds, and significant pathway enrichment analysis is performed. A total of 769 compounds are identified through metabolomics analysis, with alkaloids being predominant, followed by lipids and lipid molecules. Significant differential metabolites were screened out based on VIP > 1 and p-value < 0.05 criteria, followed by KEGG enrichment analysis of these differential metabolites. Differential metabolites between Pinelliae Rhizoma and Typhonium flagelliforme, as well as between Pinelliae Rhizoma and Pinellia pedatisecta, are significantly enriched in the biosynthesis of amino acids and protein digestion and absorption pathways. Differential metabolites between Pinelliae Rhizoma and Arisaema erubescens are mainly enriched in tyrosine metabolism and phenylalanine metabolism pathways. These findings aim to provide valuable data support and theoretical references for further research on the pharmacological substances, resource development and utilization, and quality control of Pinelliae Rhizoma.
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Fiorentino, Marika, Simona Piccolella, Claudia Gravina, Adriano Stinca, Assunta Esposito, Michelina Catauro, and Severina Pacifico. "Encapsulating Calendula arvensis (Vaill.) L. Florets: UHPLC-HRMS Insights into Bioactive Compounds Preservation and Oral Bioaccessibility." Molecules 28, no. 1 (December 26, 2022): 199. http://dx.doi.org/10.3390/molecules28010199.
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Wild edible plants, once consumed in times of famine or for health purposes, today represent an interesting dietary supplement, aimed at enriching local dishes and/or formulating healthy nutraceutical products. In fact, the broad content of different, and diversely bioactive, specialized metabolites therein suggests new scenarios of use which, in order to be as functional as possible, must maximize the bioactivity of these compounds while preserving their chemistry. In this context, based on a recent investigation on the metabolic profile of the organs of Calendula arvensis that highlighted that florets are abundant in flavonol glycosides and triterpene saponins, the freeze-drying encapsulation of their alcoholic extract (FE) into maltodextrin (MD) was investigated. FE-MD chemical composition was evaluated using Fourier Transform InfraRed spectroscopy (FTIR), while ultra-high performance liquid chromatography coupled with high-resolution tandem mass spectrometry (UHPLC-HRMS/MS) techniques were employed to unravel FE compound preservation also during in vitro simulated digestion. The establishment of H-bonds between FE compounds and MD hydroxyl groups was in line with FE-MD biocompatibility in Caco-2 cells, while in vitro digestion mostly affected structural integrity and/or diversity. Flavonol compounds underwent deglycosylation and demethylation, while deacylation, beyond oxidation, involved triterpene saponins, which massively preserve their aglycone core.
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Sypalov, S. A., N. V. Ul’yanovskii, D. S. Kosyakov, and A. T. Lebedev. "Determination of Umifenovir and Its Metabolites by High-Performance Liquid Chromatography with Combined Mass Spectrometric Detection." Журнал аналитической химии 78, no. 9 (September 1, 2023): 856–64. http://dx.doi.org/10.31857/s0044450223090153.
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An approach to the highly sensitive and selective determination of the bromine-containing antiviral drug umifenovir (Arbidol) and its metabolites in natural and waste water, activated sludge, and bottom sediments by chromatography-mass spectrometry based on a combination of two techniques– inductively coupled plasma mass spectrometry (ICP MS) and electrospray ionization high-resolution mass spectrometry (ESI HRMS) is developed. Reversed-phase chromatographic separation and detection based on ESI HRMS provide the reliable detection and identification of analytes in complex matrices, while the use of ICP-MS with 79Br signal detection makes it possible to exclude matrix effects and use a single analytical standard for quantitative analysis. The use of solid-phase extraction and pressurized liquid extraction as sample preparation methods made it possible to achieve limits of detection at a level of 0.2 ng/L and 2 µg/kg for liquid and solid samples, respectively. The developed approach was successfully tested in the analysis of real samples. It is shown that the concentrations of analytes in urban wastewaters are in the range 4.4–260 ng/L. The highest concentration (up to 3.7 mg/kg) is characteristic of activated sludge, which acts as an effective sorbent for umifenovir and its transformation products.
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Bechynska, Kamila, Jiri Sedlak, Leos Uttl, Vit Kosek, Petra Vackova, Vladimir Kocourek, and Jana Hajslova. "Metabolomics on Apple (Malus domestica) Cuticle—Search for Authenticity Markers." Foods 13, no. 9 (April 24, 2024): 1308. http://dx.doi.org/10.3390/foods13091308.
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The profile of secondary metabolites present in the apple cuticular layer is not only characteristic of a particular apple cultivar; it also dynamically reflects various external factors in the growing environment. In this study, the possibility of authenticating apple samples by analyzing their cuticular layer extracts was investigated. Ultra-high-performance liquid chromatography coupled with high-resolution tandem mass spectrometry (UHPLC-HRMS/MS) was employed for obtaining metabolomic fingerprints. A total of 274 authentic apple samples from four cultivars harvested in the Czech Republic and Poland between 2020 and 2022 were analyzed. The complex data generated, processed using univariate and multivariate statistical methods, enabled the building of classification models to distinguish apple cultivars as well as their geographical origin. The models showed very good performance in discriminating Czech and Polish samples for three out of four cultivars: “Gala”, “Golden Delicious” and “Idared”. Moreover, the validity of the models was tested over several harvest seasons. In addition to metabolites of the triterpene biosynthetic pathway, the diagnostic markers were mainly wax esters. “Jonagold”, which is known to be susceptible to mutations, was the only cultivar for which an unambiguous classification of geographical origin was not possible.
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Roy-Lachapelle, Audrey, Morgan Solliec, Sébastien Sauvé, and Christian Gagnon. "A Data-Independent Methodology for the Structural Characterization of Microcystins and Anabaenopeptins Leading to the Identification of Four New Congeners." Toxins 11, no. 11 (October 26, 2019): 619. http://dx.doi.org/10.3390/toxins11110619.
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Toxin-producing cyanobacteria are responsible for the presence of hundreds of bioactive compounds in aquatic environments undergoing increasing eutrophication. The identification of cyanotoxins is still emerging, due to the great diversity of potential congeners, yet high-resolution mass spectrometry (HRMS) has the potential to deepen this knowledge in aquatic environments. In this study, high-throughput and sensitive on-line solid-phase extraction ultra-high performance liquid chromatography (SPE-UHPLC) coupled to HRMS was applied to a data-independent acquisition (DIA) workflow for the suspect screening of cyanopeptides, including microcystin and anabaenopeptin toxin classes. The unambiguous characterization of 11 uncommon cyanopeptides was possible using a characterization workflow through extensive analysis of fragmentation patterns. This method also allowed the characterization of four unknown cyanotoxins ([Leu1, Ser7] MC-HtyR, [Asp3]MC-RHar, AP731, and AP803). The quantification of 17 common cyanotoxins along with the semi-quantification of the characterized uncommon cyanopeptides resulted with the identification of 23 different cyanotoxins in 12 lakes in Canada, United Kingdom and France. The concentrations of the compounds varied between 39 and 41,000 ng L−1. To our knowledge, this is the first DIA method applied for the suspect screening of two families of cyanopeptides simultaneously. Moreover, this study shows the great diversity of cyanotoxins in lake water cyanobacterial blooms, a growing concern in aquatic systems.
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Lefebvre, Donatien, Kevin Blanco-Valle, Jacques-Antoine Hennekinne, Stéphanie Simon, François Fenaille, François Becher, and Yacine Nia. "Multiplex Detection of 24 Staphylococcal Enterotoxins in Culture Supernatant Using Liquid Chromatography Coupled to High-Resolution Mass Spectrometry." Toxins 14, no. 4 (March 31, 2022): 249. http://dx.doi.org/10.3390/toxins14040249.
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Staphylococcal food poisoning outbreaks are caused by the ingestion of food contaminated with staphylococcal enterotoxins (SEs). Among the 27 SEs described in the literature to date, only a few can be detected using immuno-enzymatic-based methods that are strongly dependent on the availability of antibodies. Liquid chromatography, coupled to high-resolution mass spectrometry (LC-HRMS), has, therefore, been put forward as a relevant complementary method, but only for the detection of a limited number of enterotoxins. In this work, LC-HRMS was developed for the detection and quantification of 24 SEs. A database of 93 specific signature peptides and LC-HRMS parameters was optimized using sequences from 24 SEs, including their 162 variants. A label-free quantification protocol was established to overcome the absence of calibration standards. The LC-HRMS method showed high performance in terms of specificity, sensitivity, and accuracy when applied to 49 enterotoxin-producing strains. SE concentrations measured depended on both SE type and the coagulase-positive staphylococci (CPS) strain. This study indicates that LC-MS is a relevant alternative and complementary tool to ELISA methods. The advantages of LC-MS clearly lie in both the multiplex analysis of a large number of SEs, and the automated analysis of a high number of samples.
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Rocchetti, Gabriele, Francesca Ghilardelli, Paolo Bonini, Luigi Lucini, Francesco Masoero, and Antonio Gallo. "Changes of Milk Metabolomic Profiles Resulting from a Mycotoxins-Contaminated Corn Silage Intake by Dairy Cows." Metabolites 11, no. 8 (July 23, 2021): 475. http://dx.doi.org/10.3390/metabo11080475.
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In this study, an untargeted metabolomics approach based on ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS) was used for investigating changes in chemical profiles of cow milk considering diets based on mycotoxins-contaminated corn silages. For this purpose, 45 milk samples were classified into five clusters according to the corn silage contamination profile, namely (1) low levels of Aspergillus- and Penicillium-mycotoxins; (2) low levels of fumonisins and other Fusarium-mycotoxins; (3) high levels of Aspergillus-mycotoxins; (4) high levels of non-regulated Fusarium-mycotoxins; (5) high levels of fumonisins and their metabolites, and subsequently analyzed by UHPLC-HRMS followed by a multivariate statistical analysis (both unsupervised and supervised statistical approaches). Overall, the milk metabolomic profile highlighted potential correlations between the quality of contaminated corn silages (as part of the total mixed ration) and milk composition. Metabolomics allowed to identify 628 significant milk metabolites as affected by the five levels of corn silage contamination considered, with amino acids and peptides showing the highest metabolite set enrichment (134 compounds). Additionally, 78 metabolites were selected as the best discriminant of the prediction model built, possessing a variable importance in projection score >1.2. The average Log Fold-Change variations of the discriminant metabolites provided evidence that sphingolipids, together with purine and pyrimidine-derived metabolites were the most affected chemical classes. Also, metabolomics revealed a significant accumulation of oxidized glutathione in milk samples belonging to the silage cluster contaminated by emerging Aspergillus toxins, likely involved in the oxidative imbalance. These preliminary findings provide new insights into the potential role of milk metabolomics to provide chemical indicators of mycotoxins-contaminated corn silage feeding systems.
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Custodio-Mendoza, Jorge A., Havva Aktaş, Magdalena Zalewska, Jarosław Wyrwisz, and Marcin A. Kurek. "A Review of Quantitative and Topical Analysis of Anthocyanins in Food." Molecules 29, no. 8 (April 11, 2024): 1735. http://dx.doi.org/10.3390/molecules29081735.
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Anthocyanins, a subclass of flavonoids known for their vibrant colors and health-promoting properties, are pivotal in the nutritional science and food industry. This review article delves into the analytical methodologies for anthocyanin detection and quantification in food matrices, comparing quantitative and topical techniques. Quantitative methods, including High-performance Liquid Chromatography (HPLC) and Mass Spectrometry (MS), offer precise quantification and profiling of individual anthocyanins but require sample destruction, limiting their use in continuous quality control. Topical approaches, such as Near-infrared Spectroscopy (NIR) and hyperspectral imaging, provide rapid, in situ analysis without compromising sample integrity, ideal for on-site food quality assessment. The review highlights the advancements in chromatographic techniques, particularly Ultra-high-performance Liquid Chromatography (UHPLC) coupled with modern detectors, enhancing resolution and speed in anthocyanin analysis. It also emphasizes the growing importance of topical techniques in the food industry for their efficiency and minimal sample preparation. By examining the strengths and limitations of both analytical realms, this article aims to shed light on current challenges and prospective advancements, providing insights into future research directions for improving anthocyanin analysis in foods.
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Long, Solida, Izadora L. Furlani, Juliana M. de Oliveira, Diana I. S. P. Resende, Artur M. S. Silva, Luís Gales, José A. Pereira, et al. "Determination of the Absolute Configuration of Bioactive Indole-Containing Pyrazino[2,1-b]quinazoline-3,6-diones and Study of Their In Vitro Metabolic Profile." Molecules 26, no. 16 (August 21, 2021): 5070. http://dx.doi.org/10.3390/molecules26165070.
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In recent decades, fungi-derived naturally occurring quinazolines have emerged as potential drug candidates. Nevertheless, most studies are conducted for bioactivity assays, and little is known about their absorption, distribution, metabolism, and elimination (ADME) properties. To perform metabolic studies, the synthesis of the naturally occurring quinazolinone, fiscalin B (1), and its chloro derivative, 4-((1H-indol-3-yl)methyl)-8,10-dichloro-1-isobutyl-1,2-dihydro-6H-pyrazino[2,1-b]quinazoline-3,6(4H)-dione (2), disclosed as an antibacterial agent, was performed in a gram scale using a microwave-assisted polycondensation reaction with 22% and 17% yields, respectively. The structure of the non-natural (+)-fiscalin B was established, for the first time, by X-ray crystallography as (1R,4S)-1, and the absolute configuration of the naturally occurring fiscalin B (-)-1 was confirmed by comparison of its calculated and experimental electronic circular dichroism (ECD) spectra as (1S,4R)-1. in vitro metabolic studies were monitored for this class of natural products for the first time by ultra-high-performance liquid chromatography (UHPLC) coupled with high-resolution mass spectrometry (HRMS). The metabolic characteristics of 1 and 2 in human liver microsomes indicated hydration and hydroxylation mass changes introduced to the parent drugs.
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Konak, Ü. İ., H. A. Yatmaz, Ş. Nilüfer, T. Erkaymaz, and M. Certel. "Multiresidue method for the simultaneous analysis of antibiotics and mycotoxins in feeds by ultra-high performance liquid chromatography coupled to tandem mass spectrometry." Acta Alimentaria 50, no. 1 (March 5, 2021): 74–82. http://dx.doi.org/10.1556/066.2020.00159.
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AbstractResidues in animal feeds and foods of animal origin have been important safety issue concerning both human and animal health. A multiresidue method for determination of eight mycotoxins and ten antibiotics was developed and validated in animal feeds by using QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction followed by UHPLC-MS/MS. Optimisation of UHPLC-MS/MS parameters was performed to achieve good separation and resolution. The method was validated according to the European Commission Decision 2002/657/EC. Matrix matched calibration curves showed good r2 (≥0.995) values, and limit of quantification (LOQ) values varied between 1.2 and 5.2 μg kg−1. Average recoveries ranged from 60 to 102% with relative standard deviations of 2.2 and 15.6% for all type of feed samples except for tetracyclines, lincomycin, tylosin, ochratoxin A, and fumonisin (B1 and B2).
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Azzi, Mira, Sylvain Ravier, Assem Elkak, Bruno Coulomb, and Jean-Luc Boudenne. "Fast UHPLC-MS/MS for the Simultaneous Determination of Azithromycin, Erythromycin, Fluoxetine and Sotalol in Surface Water Samples." Applied Sciences 11, no. 18 (September 8, 2021): 8316. http://dx.doi.org/10.3390/app11188316.
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Chromatographic development for the determination of pharmaceuticals in environmental water samples is particularly challenging when the analytes have significantly different physico-chemical properties (solubility, polarity, pKa) often requiring multiple chromatographic methods for each active component. This paper presents a method for the simultaneous determination of azithromycin, erythromycin (antibiotics), fluoxetine (anti-depressant) and sotalol (b-blocker) in surface waters by ultra-high-performance liquid chromatography coupled with ultra-high-resolution time-of-flight mass spectrometry. These pharmaceuticals—presenting a broad spectrum of polarity (0.24 ≤ log Kow ≤ 4.05)—were separated on a C-18 analytical column, after a simple filtration step for freshwater samples or after a liquid–liquid extraction with Methyl-tertio-butyl ether (MTBE) for seawater samples. The optimized separation method (in terms of nature of column and eluent, elution gradient, and of mass spectrometric parameters), enable one to reach limits of detection ranging between 2 and 7 ng L−1 and limits of quantification between 7 and 23 ng L−1 for the four targeted molecules, within a three minute run. This method was validated using samples collected from three different surface waters in Lebanon (freshwater and seawater) and analytical results were compared with those obtained in surface waters sampled in a French river, equivalent in terms of human activities. Using this method, we report the highest concentration of pharmaceuticals found in surface water (up to 377 ng L−1 and 268 ng L−1, respectively, for azithromycin and erythromycin, in the Litani river, Lebanon).
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Hamani, Vincent, Pascaline Ory, Pierre-Edouard Bodet, Laurence Murillo, and Marianne Graber. "Untargeted Metabolomics Reveals a Complex Impact on Different Metabolic Pathways in Scallop Mimachlamys varia (Linnaeus, 1758) after Short-Term Exposure to Copper at Environmental Dose." Metabolites 11, no. 12 (December 11, 2021): 862. http://dx.doi.org/10.3390/metabo11120862.
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Ports are a good example of how coastal environments, gathering a set of diverse ecosystems, are subjected to pollution factors coming from human activities both on land and at sea. Among them, trace element as copper represents a major factor. Abundant in port ecosystem, copper is transported by runoff water and results from diverse port features (corrosion of structures, fuel, anti-fouling products, etc.). The variegated scallop Mimachlamys varia is common in the Atlantic port areas and is likely to be directly influenced by copper pollution, due to its sessile and filtering lifestyle. Thus, the aim of the present study is to investigate the disruption of the variegated scallop metabolism, under a short exposure (48 h) to a copper concentration frequently encountered in the waters of the largest marina in Europe (82 μg/L). For this, we chose a non-targeted metabolomic approach using ultra-high performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS), offering a high level of sensitivity and allowing the study without a priori of the entire metabolome. We described 28 metabolites clearly modulated by copper. They reflected the action of copper on several biological functions such as osmoregulation, oxidative stress, reproduction and energy metabolism.
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Castaldo, Luigi, Giulia Graziani, Anna Gaspari, Luana Izzo, Josefa Tolosa, Yelko Rodríguez-Carrasco, and Alberto Ritieni. "Target Analysis and Retrospective Screening of Multiple Mycotoxins in Pet Food Using UHPLC-Q-Orbitrap HRMS." Toxins 11, no. 8 (July 24, 2019): 434. http://dx.doi.org/10.3390/toxins11080434.
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A comprehensive strategy combining a quantitative method for 28 mycotoxins and a post-target screening for other 245 fungal and bacterial metabolites in dry pet food samples were developed using an acetonitrile-based extraction and an ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) method. The proposed method showed satisfactory validation results according to Commission Decision 2002/657/EC. Average recoveries from 72 to 108% were obtained for all studied mycotoxins, and the intra-/inter-day precision were below 9 and 14%, respectively. Results showed mycotoxin contamination in 99% of pet food samples (n = 89) at concentrations of up to hundreds µg/kg, with emerging Fusarium mycotoxins being the most commonly detected mycotoxins. All positive samples showed co-occurrence of mycotoxins with the simultaneous presence of up to 16 analytes per sample. In the retrospective screening, up to 54 fungal metabolites were tentatively identified being cyclopiazonic acid, paspalitrem A, fusaric acid, and macrosporin, the most commonly detected analytes.
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Rubio, Laura, Carmen Garcia-Jares, and Marta Lores. "High-Resolution Mass Spectrometry for the Comprehensive Characterization of Plant-Pigment-Based Tattoos and Dyes Formulations." Cosmetics 8, no. 2 (June 21, 2021): 55. http://dx.doi.org/10.3390/cosmetics8020055.
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There has been little research on emerging natural-pigment-based temporary tattoos and their constituents so far. This study focused on the characterization of natural henna and jagua tattoos and dyes in commercial samples. Sample manipulation and treatment were minimal to analyze natural pigments as they are marketed. The characterization of active compounds was performed by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS). A novel untargeted characterization was also applied for these types of samples, searching for compounds ranging from the original ingredients to other additives of interest they may contain. The fact that these products may also be a source of unlabelled allergens was considered. This work showed that not all of the 34 samples analyzed contained their characteristic active ingredients, and in addition, 70 substances of a different nature were found. Therefore, a rapid and high-throughput methodology has been developed for the identification of the components of these dyes, providing a necessary approach for quality control or identification of suspicious substances.
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Lee, Hyun-Jeoung, Chansik Kim, Hong-Duck Ryu, Eu Gene Chung, Dongseok Shin, and Jae Kwan Lee. "Simultaneous Determination of Pesticides and Veterinary Pharmaceuticals in Environmental Water Samples by UHPLC–Quadrupole-Orbitrap HRMS Combined with On-Line Solid-Phase Extraction." Separations 7, no. 1 (February 21, 2020): 14. http://dx.doi.org/10.3390/separations7010014.
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Pesticides and veterinary pharmaceuticals are used for effective crop production and prevention of livestock diseases; these chemicals are released into the environment via various pathways. Although the chemicals are typically present in trace amounts post-release, they could disturb aquatic ecosystems and public health through resistance development toward drugs or diseases, e.g., reproductive disorders. Thus, the residues of pesticides and veterinary pharmaceuticals in the environment must be managed and monitored. To that end, we developed a simultaneous analysis method for 41 target chemicals in environmental water samples using ultra-high-performance liquid chromatography (UHPLC)–quadrupole-orbitrap high-resolution mass spectrometry (HRMS) coupled with an on-line solid-phase extraction system. Calibration curves for determining linearity were constructed for 10–750 ng∙L−1, and the coefficient of determination for each chemical exceeded 0.99. The method’s detection and quantitation limits were 0.32–1.72 ng∙L−1 and 1.02–5.47 ng∙L−1, respectively. The on-line solid-phase extraction system exhibited excellent method reproducibility and reduced experimental error. As the proposed method is applicable to the monitoring of pesticides and veterinary pharmaceuticals in surface water and groundwater samples acquired near agricultural areas, it allows for the management of chemicals released into the environment.
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Hamany Djande, Claude Y., Paul A. Steenkamp, Lizelle A. Piater, Fidele Tugizimana, and Ian A. Dubery. "Hordatines and Associated Precursors Dominate Metabolite Profiles of Barley (Hordeum vulgare L.) Seedlings: A Metabolomics Study of Five Cultivars." Metabolites 12, no. 4 (March 31, 2022): 310. http://dx.doi.org/10.3390/metabo12040310.
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In the process of enhancing crop potential, metabolomics offers a unique opportunity to biochemically describe plant metabolism and to elucidate metabolite profiles that govern specific phenotypic characteristics. In this study we report an untargeted metabolomic profiling of shoots and roots of barley seedlings performed to reveal the chemical makeup therein at an early growth stage. The study was conducted on five cultivars of barley: ‘Overture’, ‘Cristalia’, ‘Deveron’, ‘LE7′ and ‘Genie’. Seedlings were grown for 16 days post germination under identical controlled conditions, and methanolic extracts were analysed on an ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC–HRMS) system. In addition, an unsupervised pattern identification technique, principal component analysis (PCA), was performed to process the generated multidimensional data. Following annotation of specific metabolites, several classes were revealed, among which phenolic acids represented the largest group in extracts from both shoot and root tissues. Interestingly, hordatines, barley-specific metabolites, were not found in the root tissue. In addition, metabolomic profiling revealed metabolites potentially associated with the plants’ natural protection system against potential pathogens. The study sheds light on the chemical composition of barley at a young developmental stage and the information gathered could be useful in plant research and biomarker-based breeding programs.