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1
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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Szulc, Justyna, Małgorzata Okrasa, Katarzyna Majchrzycka, Michael Sulyok, Adriana Nowak, Tomasz Ruman, Joanna Nizioł, Bogumiła Szponar, and Beata Gutarowska. "Microbiological and Toxicological Hazards in Sewage Treatment Plant Bioaerosol and Dust." Toxins 13, no. 10 (September 28, 2021): 691. http://dx.doi.org/10.3390/toxins13100691.
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Despite the awareness that work in the sewage treatment plant is associated with biological hazards, they have not been fully recognised so far. The research aims to comprehensively evaluate microbiological and toxicological hazards in the air and settled dust in workstations in a sewage treatment plant. The number of microorganisms in the air and settled dust was determined using the culture method and the diversity was evaluated using high-throughput sequencing. Endotoxin concentration was assessed with GC-MS (gas chromatography-mass spectrometry) while secondary metabolites with LC-MS/MS (liquid chromatography coupled to tandem mass spectrometry). Moreover, cytotoxicity of settled dust against a human lung epithelial lung cell line was determined with the MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay and UHPLC-Q-ToF-UHRMS (ultra-high-performance liquid chromatography-quadrupole time-of-flight ultrahigh-resolution mass spectrometry) analysis was performed to determine the source of cytotoxicity. The total dust concentration in the sewage treatment plant was low and ranged from 0.030 mg m−3 to 0.044 mg m−3. The highest microbiological contamination was observed in sludge thickening building and screenings storage. Three secondary metabolites were detected in the air and sixteen in the settled dust. They were dominated by compounds typical of lichen and plants and Aspergillus, Penicillium and Fusarium genera mould. The settled dust from the sludge thickening building revealed high cytotoxicity to human lung epithelial cells A-549 (IC50 = 6.98 after 72 h). This effect can be attributed to a biocidal compound—didecyldimethylammonium chloride (DDAC-C10) and seven toxic compounds: 4-hydroxynonenal, carbofuran, cerulenin, diethylphosphate, fenpropimorph, naphthalene and onchidal. The presence of DDAC-C10 and other biocidal substances in the sewage treatment plant environment may bring negative results for biological sewage treatment and the natural environment in the future and contribute to microorganisms’ increasing antibiotics resistance. Therefore, the concentration of antibiotics, pesticides and disinfectants in sewage treatment plant workstations should be monitored.
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Dahibhate, Nilesh Lakshman, and Kundan Kumar. "Metabolite profiling of Bruguiera cylindrica reveals presence of potential bioactive compounds." PeerJ Analytical Chemistry 4 (May 4, 2022): e16. http://dx.doi.org/10.7717/peerj-achem.16.
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Bruguiera cylindrica parts are commonly used in Chinese and Indian traditional medicine to treat diarrhea, fever, and many ailments. The present study aims non targeted analysis of key secondary metabolites of B. cylindrica by gas chromatography mass spectrometry (GC-MS) and ultra-high performance liquid chromatography hybrid quadrupole-Exactive-Orbitrap high resolution mass spectrometry (UHPLC-Q-Exactive Orbitrap HRMS). GC-MS and UHPLC-Q-Exactive Orbitrap HRMS were utilized for metabolic profiling of ethyl acetate extract of B. cylindrica leaves. Key metabolites in the extract were identified and predicted based on chemical similarity using online databases such as ChemSpider and mzCloud. Thirty-six compounds belonging to different classes of secondary metabolites viz. flavonoids, fatty acids, fatty acid amides, carboxylic acids, and alkaloids were identified in the extract. Pentacyclic triterpenes like betulin, ursolic acid and a tropine, an alkaloid with potential pharmacological and therapeutic activities such as anticancer properties, neuromuscular blockers and antioxidants, were also identified. This study combined GC-MS and UHPLC-Q-Exactive Orbitrap HRMS with available online database for effective and rapid identification of bioactive metabolites in the ethyl acetate extract of mangrove without individual standard application. This is the first report on the HRMS based secondary metabolic profiling of B. cylindrica, with comprehensive map of its biologically important metabolites.
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La Maida, Nunzia, Manuela Pellegrini, Esther Papaseit, Clara Pérez-Mañá, Lourdes Poyatos, Mireia Ventura, Liliana Galindo, et al. "Determination of the Synthetic Cannabinoids JWH-122, JWH-210, UR-144 in Oral Fluid of Consumers by GC-MS and Quantification of Parent Compounds and Metabolites by UHPLC-MS/MS." International Journal of Molecular Sciences 21, no. 24 (December 10, 2020): 9414. http://dx.doi.org/10.3390/ijms21249414.
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The consumption of synthetic cannabinoids (SCs) has significantly increased in the last decade and the analysis of SCs and their metabolites in human specimens is gaining interest in clinical and forensic toxicology. A pilot study has been carried out using a combination of an initial last generation gas chromatography-mass spectrometry (GC-MS) screening method for the determination of JWH-122, JWH-210, UR-144) in oral fluid (OF) of consumers and an ultra-high performance liquid chromatography high resolution mass spectrometry (UHPLC-HRMS) confirmatory method for the quantification of the parent compounds and their metabolites in the same biological matrix. OF samples were simply liquid-liquid extracted before injecting in both chromatographic systems. The developed methods have been successfully validated and were linear from limit of quantification (LOQ) to 50 ng/mL OF. Recovery of analytes was always higher than 70% and matrix effect always lower than 15% whereas intra-assay and inter-assay precision and accuracy were always better than 16%. After smoking 1 mg JWH-122 or UR-144 and 3 mg JWH-210, maximum concentration of 4.00–3.14 ng/mL JWH-122, 8.10–7.30 ng/mL JWH-210 ng/mL and 7.40 and 6.81 ng/mL UR-144 were measured by GC-MS and UHPLC-HRMS respectively at 20 min after inhalation. Metabolites of JWH 122 and 210 were quantified in OF by UHPLC-HRMS, while that of UR144 was only detectable in traces. Our results provide for the first time information about disposition of these SCs and their metabolites in consumers OF. Last generation GC-MS has proven useful tool to identify and quantify parent SCs whereas UHPLC-HRMS also confirmed the presence of SCs metabolites in the OF of SCs consumers.
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Rubić, Ivana, Richard Burchmore, Stefan Weidt, Clement Regnault, Josipa Kuleš, Renata Barić Rafaj, Tomislav Mašek, et al. "Multi Platforms Strategies and Metabolomics Approaches for the Investigation of Comprehensive Metabolite Profile in Dogs with Babesia canis Infection." International Journal of Molecular Sciences 23, no. 3 (January 29, 2022): 1575. http://dx.doi.org/10.3390/ijms23031575.
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Canine babesiosis is an important tick-borne disease worldwide, caused by parasites of the Babesia genus. Although the disease process primarily affects erythrocytes, it may also have multisystemic consequences. The goal of this study was to explore and characterize the serum metabolome, by identifying potential metabolites and metabolic pathways in dogs naturally infected with Babesia canis using liquid and gas chromatography coupled to mass spectrometry. The study included 12 dogs naturally infected with B. canis and 12 healthy dogs. By combining three different analytical platforms using untargeted and targeted approaches, 295 metabolites were detected. The untargeted ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) metabolomics approach identified 64 metabolites, the targeted UHPLC-MS/MS metabolomics approach identified 205 metabolites, and the GC-MS metabolomics approach identified 26 metabolites. Biological functions of differentially abundant metabolites indicate the involvement of various pathways in canine babesiosis including the following: glutathione metabolism; alanine, aspartate, and glutamate metabolism; glyoxylate and dicarboxylate metabolism; cysteine and methionine metabolism; and phenylalanine, tyrosine, and tryptophan biosynthesis. This study confirmed that host–pathogen interactions could be studied by metabolomics to assess chemical changes in the host, such that the differences in serum metabolome between dogs with B. canis infection and healthy dogs can be detected with liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) methods. Our study provides novel insight into pathophysiological mechanisms of B. canis infection.
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Marchei, Emilia, Maria Alias Ferri, Marta Torrens, Magí Farré, Roberta Pacifici, Simona Pichini, and Manuela Pellegrini. "Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry and High-Sensitivity Gas Chromatography-Mass Spectrometry Screening of Classic Drugs and New Psychoactive Substances and Metabolites in Urine of Consumers." International Journal of Molecular Sciences 22, no. 8 (April 13, 2021): 4000. http://dx.doi.org/10.3390/ijms22084000.
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The use of the new psychoactive substances is continuously growing and the implementation of accurate and sensible analysis in biological matrices of users is relevant and fundamental for clinical and forensic purposes. Two different analytical technologies, high-sensitivity gas chromatography-mass spectrometry (GC-MS) and ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) were used for a screening analysis of classic drugs and new psychoactive substances and their metabolites in urine of formed heroin addicts under methadone maintenance therapy. Sample preparation involved a liquid-liquid extraction. The UHPLC-HRMS method included Accucore™ phenyl Hexyl (100 × 2.1 mm, 2.6 μm, Thermo, USA) column with a gradient mobile phase consisting of mobile phase A (ammonium formate 2 mM in water, 0.1% formic acid) and mobile phase B (ammonium formate 2 mM in methanol/acetonitrile 50:50 (v/v), 0.1% formic acid) and a full-scan data-dependent MS2 (ddMS2) mode for substances identification (mass range 100–1000 m/z). The GC-MS method employed an ultra-Inert Intuvo GC column (HP-5MS UI, 30 m, 250 µm i.d, film thickness 0.25 µm; Agilent Technologies, Santa Clara, CA, USA) and electron-impact (EI) mass spectra were recorded in total ion monitoring mode (scan range 40–550 m/z). Urine samples from 296 patients with a history of opioid use disorder were examined. Around 80 different psychoactive substances and/or metabolites were identified, being methadone and metabolites the most prevalent ones. The possibility to screen for a huge number of psychotropic substances can be useful in suspected drug related fatalities or acute intoxication/exposure occurring in emergency departments and drug addiction services.
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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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Pellegrini, Manuela, Emilia Marchei, Esther Papaseit, Magí Farré, and Simona Zaami. "UHPLC-HRMS and GC-MS Screening of a Selection of Synthetic Cannabinoids and Metabolites in Urine of Consumers." Medicina 56, no. 8 (August 13, 2020): 408. http://dx.doi.org/10.3390/medicina56080408.
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Background and Objectives: The use of synthetic cannabinoids has increased around the world. As a result, the implementation of accurate analysis in human biological matrices is relevant and fundamental. Two different analytical technologies, ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) and high-sensitivity gas chromatography-mass spectrometry (GC-MS) were used for the determination of three synthetic cannabinoids JWH-122, JWH 210, UR-144 and their metabolites in urine of consumers. Materials and Methods: Sample preparation included an initial hydrolysis with β-glucuronidase and liquid-liquid extraction. The UHPLC-HRMS method included a Kinetex 2.6 u Biphenyl 100A (100 × 2.1 mm, 2.6 μm) (Phenomenex, Italy) column with a gradient mobile phase consisting of mobile phase A (ammonium formate 2mM in water, 0.1% formic acid) and mobile phase B (ammonium formate 2mM in methanol/acetonitrile 50:50 (v/v), 0.1% formic acid) and a full-scan data-dependent MS2 (ddMS2) mode was used (mass range 100–1000 m/z). The GC-MS method employed an ultra-Inert Intuvo GC column (HP-5MS UI, 30 m × 250 µm i.d, film thickness 0.25 µm; Agilent Technologies, Santa Clara, CA, USA) and electron-impact (EI) mass spectra were recorded in total ion monitoring mode (scan range 40–550 m/z). Results: Both methods have been successfully used for screening of parent synthetic cannabinoids and their metabolites in urine samples of consumers. Conclusions: The screening method applied JWH-122, JWH-210, UR-144 and their metabolites in urine of consumers can be applied to other compounds of the JWH family.
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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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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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Theofel, Nadine, Marlene Wagner, Elke Vejmelka, Stefan Scholtis, and Michael Tsokos. "Herbal Medicine Must Be Treated with Care—A Case Report on Aconitine." Forensic Sciences 1, no. 1 (May 5, 2021): 25–32. http://dx.doi.org/10.3390/forensicsci1010005.
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Pathologists usually only request a screening for natural toxic substances if plant material has been observed during autopsy or if there exists a hint in the police investigation file. This situation is aggravated by the fact that most toxins are not covered by typical immunoassays and gas chromatography–mass spectrometry (GC–MS) profiling systems. In addition, only a few forensic toxicological libraries based on liquid chromatography coupled to high-resolution tandem mass spectrometry (LC–HRMS/MS) exist. In the following case, femoral blood and urine were applied to systematic toxicological analysis (STA). However, the concentrations determined in blood did not lead to death. Consequently, a liquid chromatography high-resolution tandem mass spectrometry (LC–HRMS/MS) screening approach was applied. Aconitine was quantitated in all specimens taken during autopsy and urine and bile fluid screened for aconitine metabolites. Aconitine, jesaconitine, hypaconitine, and mesaconitine were found in the root piece collected from the duodenum. Apart from aconitine, no other alkaloids were detected in the urine or in the femoral blood sample. The highest concentrations of aconitine were found in gastric content (55.2 μg/mL), bile fluid (11.7 μg/mL), and liver (9.14 μg/g), and least in femoral blood (0.15 μg/mL) and cerebrospinal fluid (0.07 μg/mL). The liver/peripheral blood ratio amounted to 61 L/kg and indicated that aconitine undergoes postmortem redistribution. During our metabolism investigation, we found 3-dehydrogen-aconitine in the urine and bile fluid sample and N-deethyl-aconitine only in the bile fluid sample. If the routine GC–MS screening approach does not come up with a toxin, then LC–HRMS/MS profiling could represent the method of choice. In this case aconitine was identified. The concentrations determined were compared to those reported in literature and clearly indicate that the deceased died due to an aconitine overdose.
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Hoenigsberger, Michaela, Alexey Kopchinskiy, Christoph Bueschl, Alexandra Parich, Alice Laciny, Herbert Zettel, Kamariah Salim, Linda Lim, Irina Druzhinina, and Rainer Schuhmacher. "Volatiles from the Mandibular Gland Reservoir Content of Colobopsis explodens Laciny and Zettel, 2018, Worker Ants (Hymenoptera: Formicidae)." Molecules 24, no. 19 (September 24, 2019): 3468. http://dx.doi.org/10.3390/molecules24193468.
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Forty-five volatile organic compounds (VOCs) were identified or annotated in the mandibular gland reservoir content (MGRC) of the Southeast Asian ant Colobopsis explodens Laciny and Zettel, 2018 (Hymenoptera: Formicidae), using headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography mass spectrometry (GC-MS) and liquid extraction combined with GC-MS. In extension of previous reports on VOCs of C. explodens, members of different compound classes, such as alkanes, aliphatic and aromatic carboxylic acids, and phenolics, were detected. The ketone 2-heptanone and the biochemically related phenolics benzene-1,3,5-triol (phloroglucinol, PG), 1-(2,4,6-trihydroxyphenyl)ethanone (monoacetylphloroglucinol, MAPG), 5,7-dihydroxy-2-methylchromen-4-one (noreugenin), and 1-(3-Acetyl-2,4,6-trihydroxyphenyl)ethanone (2,4-diacetylphloroglucinol, DAPG) dominated the GC-MS chromatograms. The identities of the main phenolics MAPG and noreugenin were further verified by liquid chromatography-high resolution-tandem mass spectrometry (LC-HRMS/MS). A comparative study of MGRC samples originating from three distinct field expeditions revealed differences in the VOC profiles, but the presence and relative abundances of the dominating constituents were largely consistent in all samples. Our study considerably extends the knowledge about the number and type of VOCs occurring in the MGRC of C. explodens. Based on the type of the detected compounds, we propose that the likely irritant and antibiotic phenolic constituents play a role in defense against arthropod opponents or in protection against microbial pathogens.
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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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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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Zhu, Chenglin, Xin Pan, Guo Li, Caiwu Li, Daifu Wu, Junni Tang, Yan Huang, Likou Zou, and Luca Laghi. "Lipidomics for Determining Giant Panda Responses in Serum and Feces Following Exposure to Different Amount of Bamboo Shoot Consumption: A First Step towards Lipidomic Atlas of Bamboo, Giant Panda Serum and Feces by Means of GC-MS and UHPLC-HRMS/MS." International Journal of Molecular Sciences 23, no. 19 (September 29, 2022): 11544. http://dx.doi.org/10.3390/ijms231911544.
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Lipidic metabolites play essential roles in host physiological health and growth performance, serving as the major structural and signaling components of membranes, energy storage molecules, and steroid hormones. Bamboo, as wild giant pandas’ exclusive diet, is the main determinant of giant pandas’ lipidome, both as a direct source and through microbiota activity. Interestingly, the consumption of bamboo has attracted little attention from a lipidomic perspective. In the current study, we outline the lipidomic atlas of different parts of bamboo. By gas chromatography—mass spectrometry (GC-MS), we have been able to obtain the absolute quantification of 35 fatty acids pertaining to short chain fatty acids (8), medium chain fatty acids (6), long chain fatty acids (17), and very long chain fatty acids (4), while liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS/MS) allowed us to obtain the relative quantification of another 1638 lipids. Among the fatty acids quantified in absolute terms, eight showed significantly distinct concentrations among different bamboo parts. Subsequently, we investigated how the giant panda’s serum and fecal lipidome adapt to the most important annual change in their diet, represented by the consumption of high amounts of bamboo shoots, typical of spring, the weight-gaining season. Five fatty acids were significantly altered in feces and two in serum, respectively, due to the different levels of bamboo shoot consumption. Furthermore, significant differences of the main bacteria strains were observed in feces between the two groups at the genus level, pertaining to Streptococcus, Leuconostoc, and Vagococcus. Correlations between giant panda fecal microbiome and lipidome were evaluated by Pearson correlation analysis. These findings suggest that a balanced diet, important for the overall lipidomic function and giant panda health, could be reached even in this remarkable case of a single food-based diet, by administering to the giant panda’s combinations of different parts of bamboo, with specific lipidome profiles.
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Monga, Gaganpreet Kaur, Anima Ghosal, and Dil Ramanathan. "To Develop the Method for UHPLC-HRMS to Determine the Antibacterial Potential of a Central American Medicinal Plant." Separations 6, no. 3 (July 29, 2019): 37. http://dx.doi.org/10.3390/separations6030037.
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The development of antibiotic resistance by microbials has long been acknowledged. The major challenge worldwide is to develop novel, natural, and potent antibiotics against the multidrug resistant bacteria. In this study, our aim was to develop the method for a highly sensitive instrument, ultra-high performance liquid chromatograph-high resolution mass spectrometer (UHPLC-HRMS), to evaluate the antibacterial property of a natural product. Aechmea magdalenae (Andre) Andre ex Baker, a plant belonging to the family Bromeliaceae, a native of Central America was used in this study. Based on the available literature, it was hypothesized that Aechmea magdalenae has antibacterial activity. In addition, the profiling done on A. magdalenae using gas chromatography-mass spectrometry (GC-MS) also revealed the presence of medicinally important chemical compounds, such as acetic acid. Minimum inhibitory concentration (MIC) of dried Aechmea plant extract was determined for the first time using 96-well plate assay, followed by determination of antibacterial potential using LC-MS. The reason being that other dried methanolic plant extracts, such as Vismia macrophylla, lined up for antibacterial testing have dark extracts, for which determining the antibacterial potential and reading the results with the naked eye would be challenging. To overcome the situation of dark plant extracts, a generalized novel LC-MS method was developed that was used for the plant A. magdalenae, and would be used further for other plants. A blue indicator called resazurin was added to the wells; resazurin, upon incubation with the living cells, got reduced to resorufin (which was pink), while it remained blue with bacterial growth inhibition. The mass difference created due to reduction of resazurin to resorufin was detected by using LTQ Orbitrap Discovery in positive ion mode to determine the antibacterial activity of the plant extract. The sample preparation for LC-MS assay included centrifugation of the samples taken from 96-well plate, followed by filtration of the supernatant, before exposing them to C-18 column. The results obtained from full scan LC-MS spectrum consistently demonstrated the presence of resorufin from wells with bacterial growth, and resazurin from wells with inhibition through peaks of relevant masses.
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Wang, Yuqi, Xiaodan Mei, Zihan Liu, Jie Li, Xiaoxin Zhang, Shuang Lang, Long Dai, and Jiayu Zhang. "Drug Metabolite Cluster-Based Data-Mining Method for Comprehensive Metabolism Study of 5-hydroxy-6,7,3′,4′-tetramethoxyflavone in Rats." Molecules 24, no. 18 (September 9, 2019): 3278. http://dx.doi.org/10.3390/molecules24183278.
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The screening of drug metabolites in biological matrixes and structural characterization based on product ion spectra is among the most important, but also the most challenging due to the significant interferences from endogenous species. Traditionally, metabolite detection is accomplished primarily on the basis of predicted molecular masses or fragmentation patterns of prototype drug metabolites using ultra-high performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS). Although classical techniques are well-suited for achieving the partial characterization of prototype drug metabolites, there is a pressing need for a strategy to enable comprehensive drug metabolism depiction. Therefore, we present drug metabolite clusters (DMCs), different from, but complementary to, traditional approaches for mining the information regarding drugs and their metabolites on the basis of raw, processed, or identified tandem mass spectrometry (MS/MS) data. In this paper, we describe a DMC-based data-mining method for the metabolite identification of 5-hydroxy-6,7,3′,4′-tetramethoxyflavone (HTF), a typical hydroxylated-polymethoxyflavonoid (OH-PMF), which addressed the challenge of creating a thorough metabolic profile. Consequently, eight primary metabolism clusters, sixteen secondary metabolism clusters, and five tertiary metabolism clusters were proposed and 106 metabolites (19 potential metabolites included) were detected and identified positively and tentatively. These metabolites were presumed to generate through oxidation (mono-oxidation, di-oxidation), methylation, demethylation, methoxylation, glucuronidation, sulfation, ring cleavage, and their composite reactions. In conclusion, our study expounded drug metabolites in rats and provided a reference for further research on therapeutic material basis and the mechanism of drugs.
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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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Alías-Ferri, Maria, Manuela Pellegrini, Emilia Marchei, Roberta Pacifici, Maria Concetta Rotolo, Simona Pichini, Clara Pérez-Mañá, et al. "New Psychoactive Substances Consumption in Opioid-Use Disorder Patients." Biology 11, no. 5 (April 22, 2022): 645. http://dx.doi.org/10.3390/biology11050645.
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(1) Background: Since the beginning of the 21st century, the large number and wide chemical variety of new psychoactive substances (NPS) that enter the market every year has become a public health problem. Given the rapidity with which the drug market is changing, many NPS are not clinically investigated and their effects and health risks are unknown. Drug testing is a very useful tool for this purpose, but, unfortunately, it is not very widespread in individuals with opioid-use disorder under detoxification treatment. The aim of this study is to investigate the use of illicit drugs and NPS in opioid-use disorder (OUD) patients on opioid agonist treatment. (2) Methods: A multicenter, descriptive, cross-sectional study was conducted at two addiction care services in Barcelona and Badalona, Spain. Urine samples were collected from OUD individuals attending these two centers, who anonymously donated a urine sample at the time of a periodical visit. Samples were analyzed by high-sensitivity gas chromatography-mass spectrometry (GC-MS) and ultra-high-performance liquid chromatography-high –resolution mass spectrometry (UHPLC-HRMS). (3) Results: Out of the 187 collected and analyzed urine samples, 27.3% were positive for any type of NPS and 8.6% were positive for new synthetic opioids, including fentanyl and its derivatives (NSO). Other frequently detected substances were benzodiazepines in 46.0% of samples, antipsychotics in 27.8% of samples, or cocaine and cannabis in 23.5% of samples. (4) Conclusion: A wide number of NPS, including NSO, have been detected in urine samples from an OUD population. A lack of NPS detection in standard drug screening among drug users can hide the identification of a potential public health problem.
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Manaig, Yron Joseph Yabut, Silvia Sandrini, Sara Panseri, Gabriella Tedeschi, Josep M. Folch, Armand Sánchez, Giovanni Savoini, and Alessandro Agazzi. "Low n-6/n-3 Gestation and Lactation Diets Influence Early Performance, Muscle and Adipose Polyunsaturated Fatty Acid Content and Deposition, and Relative Abundance of Proteins in Suckling Piglets." Molecules 27, no. 9 (May 4, 2022): 2925. http://dx.doi.org/10.3390/molecules27092925.
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Elevated omega-6 (n-6) and omega-3 (n-3) polyunsaturated fatty acids (PUFAs) ratios in swine diets can potentially impose a higher risk of inflammatory and metabolic diseases in swine. A low ratio between the two omega PUFAs has beneficial effects on sows’ and piglets’ production performance and immunity status. At present, there are few studies on how sow nutrition directly affects the protein and fat deposition in suckling piglets. Two groups of sows were fed diets with high or low n-6/n-3 polyunsaturated ratios of 13:1 (SOY) and 4:1 (LIN), respectively, during gestation and lactation. Longissimus dorsi muscle and adipose tissue from newborn piglets, nourished only with sow’s milk, were subjected to fatty acid profiling by gas chromatography–mass spectrometry (GC-MS) and to proteomics assays based on nano-liquid chromatography coupled to high-resolution tandem mass spectrometry (nLC-HRMS). Fatty acid profiles on both muscle and adipose tissues resembled the magnitude of the differences between fatty acid across diets. Proteomic analysis revealed overabundance of 4 muscle and 11 adipose tissue proteins in SOY compared to LIN in both piglet tissues. The detected overabundance of haptoglobin, an acute-phase protein, and the stimulation of protein-coding genes and proteins related to the innate immune response and acute inflammatory response could be associated with the pro-inflammatory role of n-6 PUFAs.
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Radman, Sanja, Martina Čagalj, Vida Šimat, and Igor Jerković. "Seasonal Monitoring of Volatiles and Antioxidant Activity of Brown Alga Cladostephus spongiosus." Marine Drugs 21, no. 7 (July 21, 2023): 415. http://dx.doi.org/10.3390/md21070415.
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Cladostephus spongiosus was harvested once a month during its growing season (from May to August) from the Adriatic Sea. Algal volatile organic compounds (VOCs) were obtained by headspace solid-phase microextraction (HS-SPME) and hydrodistillation (HD) and analysed by gas chromatography and mass spectrometry (GC-MS). The effects of air drying and growing season on VOCs were determined. Two different extraction methods (ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE)) were used to obtain ethanolic extracts of C. spongiosus. In addition, the seasonal antioxidant potential of the extracts was determined, and non-volatile compounds were identified from the most potent antioxidant extract. Aliphatic compounds (e.g., pentadecane) were predominantly found by HS-SPME/GC-MS. Hydrocarbons were more than twice as abundant in the dry samples (except in May). Aliphatic alcohols (e.g., hexan-1-ol, octan-1-ol, and oct-1-en-3-ol) were present in high percentages and were more abundant in the fresh samples. Hexanal, heptanal, nonanal, and tridecanal were also found. Aliphatic ketones (octan-3-one, 6-methylhept-5-en-2-one, and (E,Z)-octa-3,5-dien-2-one) were more abundant in the fresh samples. Benzene derivatives (e.g., benzyl alcohol and benzaldehyde) were dominant in the fresh samples from May and August. (E)-Verbenol and p-cymen-8-ol were the most abundant in dry samples in May. HD revealed aliphatic compounds (e.g., heptadecane, pentadecanal, (E)-heptadec-8-ene, (Z)-heptadec-3-ene), sesquiterpenes (germacrene D, epi-bicyclosesquiphellandrene, gleenol), diterpenes (phytol, pachydictyol A, (E)-geranyl geraniol, cembra-4,7,11,15-tetraen-3-ol), and others. Among them, terpenes were the most abundant (except for July). Seasonal variations in the antioxidant activity of the ethanolic extracts were evaluated via different assays. MAE extracts showed higher peroxyl radical inhibition activity from 55.1 to 74.2 µM TE (Trolox equivalents). The highest reducing activity (293.8 µM TE) was observed for the May sample. Therefore, the May MAE extract was analysed via high-performance liquid chromatography with high-resolution mass spectrometry and electrospray ionisation (UHPLC-ESI-HRMS). In total, 17 fatty acid derivatives, 9 pigments and derivatives, and 2 steroid derivatives were found. The highest content of pheophorbide a and fucoxanthin, as well as the presence of other pigment derivatives, could be related to the observed antioxidant activity.
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Fitzgerald, Christopher C. J., Rikard Hedman, Dimanthi R. Uduwela, Bettina Paszerbovics, Adam J. Carroll, Teresa Neeman, Adam Cawley, Lance Brooker, and Malcolm D. McLeod. "Profiling Urinary Sulfate Metabolites With Mass Spectrometry." Frontiers in Molecular Biosciences 9 (February 23, 2022). http://dx.doi.org/10.3389/fmolb.2022.829511.
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The study of urinary phase II sulfate metabolites is central to understanding the role and fate of endogenous and exogenous compounds in biological systems. This study describes a new workflow for the untargeted metabolic profiling of sulfated metabolites in a urine matrix. Analysis was performed using ultra-high-performance liquid chromatography-high resolution tandem mass spectrometry (UHPLC-HRMS/MS) with data dependent acquisition (DDA) coupled to an automated script-based data processing pipeline and differential metabolite level analysis. Sulfates were identified through k-means clustering analysis of sulfate ester derived MS/MS fragmentation intensities. The utility of the method was highlighted in two applications. Firstly, the urinary metabolome of a thoroughbred horse was examined before and after administration of the anabolic androgenic steroid (AAS) testosterone propionate. The analysis detected elevated levels of ten sulfated steroid metabolites, three of which were identified and confirmed by comparison with synthesised reference materials. This included 5α-androstane-3β,17α-diol 3-sulfate, a previously unreported equine metabolite of testosterone propionate. Secondly, the hydrolytic activity of four sulfatase enzymes on pooled human urine was examined. This revealed that Pseudomonas aeruginosa arylsulfatases (PaS) enzymes possessed higher selectivity for the hydrolysis of sulfated metabolites than the commercially available Helix pomatia arylsulfatase (HpS). This novel method provides a rapid tool for the systematic, untargeted metabolic profiling of sulfated metabolites in a urinary matrix.
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Ding, Su, Nicole J. Bale, Ellen C. Hopmans, Laura Villanueva, Milou G. I. Arts, Stefan Schouten, and Jaap S. Sinninghe Damsté. "Lipidomics of Environmental Microbial Communities. II: Characterization Using Molecular Networking and Information Theory." Frontiers in Microbiology 12 (July 12, 2021). http://dx.doi.org/10.3389/fmicb.2021.659315.
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Structurally diverse, specialized lipids are crucial components of microbial membranes and other organelles and play essential roles in ecological functioning. The detection of such lipids in the environment can reveal not only the occurrence of specific microbes but also the physicochemical conditions to which they are adapted to. Traditionally, liquid chromatography coupled with mass spectrometry allowed for the detection of lipids based on chromatographic separation and individual peak identification, resulting in a limited data acquisition and targeting of certain lipid groups. Here, we explored a comprehensive profiling of microbial lipids throughout the water column of a marine euxinic basin (Black Sea) using ultra high-pressure liquid chromatography coupled with high-resolution tandem mass spectrometry (UHPLC-HRMS/MS). An information theory framework combined with molecular networking based on the similarity of the mass spectra of lipids enabled us to capture lipidomic diversity and specificity in the environment, identify novel lipids, differentiate microbial sources within a lipid group, and discover potential biomarkers for biogeochemical processes. The workflow presented here allows microbial ecologists and biogeochemists to process quickly and efficiently vast amounts of lipidome data to understand microbial lipids characteristics in ecosystems.
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Wagmann, Lea, Sascha K. Manier, and Markus R. Meyer. "Can the Intake of a Synthetic Tryptamine be Detected Only by Blood Plasma Analysis? A Clinical Toxicology Case Involving 4-HO-MET." Journal of Analytical Toxicology, June 17, 2021. http://dx.doi.org/10.1093/jat/bkab062.
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Abstract Tryptamines represent a group of hallucinogenic new psychoactive substances with increasing prevalence. Unfortunately, only limited data concerning their toxicology and bioanalysis are available as tryptamines are not included in routine screening procedures in many laboratories. In order to expand the current knowledge, we report a non-fatal clinical toxicology case involving the synthetic tryptamine 4-HO-MET (4-hydroxy-N-methyl-N-ethyl-tryptamine, 3-{2-[ethyl(methyl)amino]ethyl}-1H-indol-4-ol, metocin or methylcybin). As only blood of the intoxicated patient was available, our systematic blood plasma screening approaches based on gas chromatography–mass spectrometry (GC–MS) and liquid chromatography (LC) coupled to low-resolution linear ion trap mass spectrometry (ITMSn) or high-resolution tandem mass spectrometry (HRMS/MS) were conducted. The ingestion of the synthetic tryptamine 4-HO-MET could be revealed by blood plasma analysis using both LC-based systematic screening approaches. However, 4-HO-MET was not detected by GC–MS. Furthermore, the detection of metabolites, which may be used to confirm an intake of the parent compound 4-HO-MET, was only successful using LC–HRMS/MS most probably due to its increased sensitivity compared to LC–ITMSn. A total of four metabolites were detected in blood, including N-demethyl-, oxo- and hydroxy-4-HO-MET, as well as the N-oxide. Finally, LC–HRMS/MS analysis revealed a plasma concentration of 193 ng/mL for 4-HO-MET using the standard addition method. The presented data may help clinical and forensic toxicologists with the interpretation of future cases involving synthetic tryptamines, especially if only blood samples are available.
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Hegazi, Nesrine, Amira R. Khattab, Hamada H. Saad, Bishoy Abib, and Mohamed A. Farag. "A multiplex metabolomic approach for quality control of Spirulina supplement and its allied microalgae (Amphora & Chlorella) assisted by chemometrics and molecular networking." Scientific Reports 14, no. 1 (February 2, 2024). http://dx.doi.org/10.1038/s41598-024-53219-5.
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AbstractMicroalgae species are of economic importance regarded as “green gold” being rich in bioactive compounds. Spirulina and Chlorella are the most popular microalgal species and are marketed as healthy food supplements. At the same time, Amphora holds potential as a source of healthy lipids and essential fatty acids. Yet, there are considerable variations in their reported chemical composition, and less is known about their compositional differences. A multiplexed metabolomic approach was adopted for the quality control (QC) of Spirulina supplements and to compare its constitutive metabolome to Chlorella and Amphora. The adopted protocol comprised gas chromatography-mass spectrometry (GC–MS), ultra-high performance liquid chromatography coupled with high-resolution tandem mass spectrometry (UPLC-HRMS/MS), and ultraviolet–visible spectrophotometry (UV/Vis) for mapping their primary and secondary metabolome. Interestingly, UPLC-HRMS/MS analysis delineated the abundance of fatty acids in Amphora versus glycolipids enrichment in Spirulina, and porphyrins were the main pigments identified in Spirulina, with scarce occurrence in Chlorella. Orthogonal projections to latent structures discriminant analysis (OPLS-DA) analysis of GC–MS data set revealed palmitic acid, 3-mannobiose, and glyceryl-glycoside as being most enriched in Spirulina, versus sucrose and leucine in Chlorella and Amphora, respectively. Despite being of low discriminatory potential, UV/Vis OPLS-DA modeling showed that Spirulina was distinguished with the UV absorbances of carotenoids and chlorophyll pigments, as indicated by its OPLS-DA derived S-plot. Our study provides a QC approach for the analysis of the microalgal species and poses alternative spectral and compositional markers for their discrimination.
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Zhang, Yanjie, Qing Zhao, Youwei Feng, Yuanhang Dong, Tianjiao Zhang, Qiu Yang, Huihui Gu, Jinyong Huang, and Yan Li. "Integrated Transcriptomic and Metabolomic Analyses Reveal the Mechanisms Underlying Anthocyanin Coloration and Aroma Formation in Purple Fennel." Frontiers in Nutrition 9 (April 27, 2022). http://dx.doi.org/10.3389/fnut.2022.875360.
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The color and aroma are the significant traits of vegetables and fruits, but the metabolic and molecular mechanisms underlying anthocyanin accumulation and aroma formation remain almost unknown in fennel (Anethum foeniculum L.), which is a crucial vegetable crop and grown widely for aromatic leaves and bulbs. Here, ten major anthocyanins identified and quantified by ultra-high performance liquid chromatography coupled with quadrupole Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) were mainly responsible for the coloration of purple fennel leaf. With the application of GC-MS, it was found that the reduced volatile phenylpropanoids including isoeugenol, trans-isoeugenol, and apiol chiefly account for the characteristic aroma changes of the purple fennel. Moreover, the characteristic anthocyanin coloration and aroma formation in purple fennel were systematically studied with the integrated transcriptomics and metabolomics. The critical genes associated with the biosynthesis and regulation of anthocyanins and volatile phenylpropanoids were isolated and studied carefully in transiently transfected tobacco cells and transgenic tomato plants. Together with the results of UHPLC-Q-Orbitrap HRMS, RT-qPCR, and yeast two hybrid (Y2H), it is proved that the metabolic flux redirection of phenylpropanoid pathway primarily regulated by a functional MYB-bHLH-WD40 complex consisting of AfTT8, AfMYB7, and AfTTG1 accounts for the characteristic anthocyanin coloration and aroma formation in purple fennel leaf. The systematic understanding of the anthocyanin accumulation and aroma formation will assist in the improvement of fennel resource utilization and breeding.
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Alías-Ferri, María, Manuela Pellegrini, Emilia Marchei, Roberta Pacifici, Maria Concetta Rotolo, Simona Pichini, Clara Pérez-Mañá, et al. "Synthetic cannabinoids use in a sample of opioid-use disorder patients." Frontiers in Psychiatry 13 (August 3, 2022). http://dx.doi.org/10.3389/fpsyt.2022.956120.
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Cannabis is the most widely consumed illegal drug in the world and synthetic cannabinoids are increasingly gaining popularity and replacing traditional cannabis. These substances are a type of new psychoactive substance that mimics the cannabis effects but often are more severe. Since, people with opioids use disorder use widely cannabis, they are a population vulnerable to use synthetic cannabinoids. In addition, these substances are not detected by the standard test used in the clinical practice and drug-checking is more common in recreational settings. A cross-sectional study with samples of 301 opioid use disorder individuals was carried out at the addiction care services from Barcelona and Badalona. Urinalysis was performed by high-sensitivity gas chromatography-mass spectrometry (GC-MS) and ultra-high-performance liquid chromatography-high –resolution mass spectrometry (UHPLC-HRMS). Any synthetic cannabinoid was detected in 4.3% of the individuals and in 23% of these samples two or more synthetic cannabinoids were detected. Among the 8 different synthetic cannabinoids detected, most common were JWH-032 and JWH-122. Natural cannabis was detected in the 18.6% of the samples and only in the 0.7% of them THC was identified. Several different synthetic cannabinoids were detected and a non-negligible percentage of natural cannabis was detected among our sample. Our results suggest that the use of synthetic cannabinoids may be related to the avoidance of detection. In the absence of methods for the detection of these substances in clinical practice, there are insufficient data and knowledge making difficult to understand about this phenomenon among opioid use disorder population.
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Jiang, Meng, Mengwen Peng, Yuxia Li, Guifang Li, Xiaobo Li, and Li Zhuang. "Quality evaluation of four Ferula plants and identification of their key volatiles based on non-targeted metabolomics." Frontiers in Plant Science 14 (January 4, 2024). http://dx.doi.org/10.3389/fpls.2023.1297449.
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IntroductionFerula is a traditional, edible, and important medicinal plant with high economic value. The distinction between edible and non-edible Ferula remains unclear.MethodsIn this study, headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry (HS-SPME/GC-MS) and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) non-targeted metabolomics techniques were used to systematically and comprehensively analyse secondary metabolites in the leaves and roots of four species of Ferula, considering their edibility.ResultsA total of 166 leaf volatile organic compounds (VOCs) and 1,079 root metabolites were identified. Additionally, 42 potential VOCs and 62 differential root metabolites were screened to distinguish between edible and non-edible Ferula. Twelve volatile metabolites were specific to F. feurlaeoides, and eight compounds were specific to the three edible Ferula species. The results showed that compounds containing sulphur, aldehydes, and ketones, which produce pungent odours, were the primary sources of the strong odour of Ferula. The root differential metabolites include 13 categories, among which the high concentration group is organic acids, amino acids, terpenoids and fatty acids. The bioactive metabolites and VOCs in the roots exhibited species-specific characteristics. VOCs with various odors were linked to the distribution of root metabolites in both edible and non-edible Ferula plants. The screened root markers may contribute to the formation of characteristic VOCs.DiscussionThis study identified the difference in flavour between edible and non-edible Ferula plants and, for the first time, demonstrated the contribution of the efficacy of Ferula root to the unique flavour of the above-ground parts of Ferula. These results provide a theoretical basis for selecting Ferula for consumption and help evaluate the quality of different species of Ferula. Our findings may facilitate food processing and the further development of Ferula.
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Ryparova Kvirencova, Jana, Klara Navratilova, Vojtech Hrbek, and Jana Hajslova. "Detection of botanical adulterants in saffron powder." Analytical and Bioanalytical Chemistry, August 17, 2023. http://dx.doi.org/10.1007/s00216-023-04853-x.
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AbstractSaffron is a unique spice obtained by drying stigmas of saffron flowers (Crocus sativus L.). Due to its high price, economically motivated adulteration occurs relatively often. The presented study aimed to develop an effective strategy for the detection of the following potential botanical adulterants used for a saffron substitution or dilution: safflower (Carthamus tinctorius L.), calendula (Calendula officinalis L.), turmeric (Curcuma longa L.), achiote (Bixa orellana L.), red pepper (Capsicum spp.), mountain arnica (Arnica montana L.), beet (Beta vulgaris L.), and pomegranate (Punica granatum L.). A non-target screening strategy based on ultra-high performance reverse-phase liquid chromatography coupled to tandem high-resolution mass spectrometry (UHPLC-HRMS/MS) was employed for the analysis of an aqueous ethanol plant extract. By using multivariate statistical methods, principal components analysis (PCA), and partial least squares discriminant analysis (PLS-DA), for processing the generated “chemical fingerprints,” metabolites unique to the investigated plants could be identified. To enable routine saffron authenticity control by target screening, an internal spectral database was developed; currently, it involves 82 unique markers. In this way, the detection addition as low as 1% (w/w) of all analyzed botanical adulterants in admixture with saffron was possible. The developed method was used to control 7 saffron powder samples from the Czech market, and none of the monitored adulterants were confirmed.
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Gunash, Jan, Juan J. Aristizabal Henao, and Ken D. Stark. "Palmitic and Stearic Free Fatty Acids Are Consistently Found in Materials used for Dried Blood Spot Collection." FASEB Journal 31, S1 (April 2017). http://dx.doi.org/10.1096/fasebj.31.1_supplement.955.13.
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BackgroundDried blood spotting has been used to collect samples for fatty acid analysis, particularly when access to analytical laboratories or ultra‐cold storage is limited. However, the materials used to collect dried blood spots are often contaminated with lipids and/or fatty acids.ObjectiveTo measure background/containment fatty acid and lipids on materials used to collect dried blood spots.MethodsThree materials used for dried blood spot collection that included 903 protein saver cards (Fischer Scientific, St. Louis, USA), chromatography paper cut into strips (Analtech Inc., Newark, DE), and novel Mitra Microsamplers (Neoteryx, California, USA). Blank collection materials as purchased were handled with nitrile gloves and preexisting lipids were extracted using 2:1 chloroform:methanol (v/v) solution. Lipid extracts were divided into two, with one portion for gas chromatography (GC) analysis of fatty acids and the other portion for lipidomic analyses using ultra‐high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC‐MS/MS) in a quadrupole‐orbitrap system (Q‐Exactive, Thermo Scientific, New York, USA). Fatty acid methyl esters were prepared for GC analysis by direct transesterification of the lipid extracts using boron trifluoride. Lipid extracts were dried and re‐suspended in 65:35:5 acetonitrile:isopropanol:water + 0.1% formic acid and analyzed using a 47‐minute reversed‐phase UHPLC multi‐step binary protocol with top‐5 data dependent MS/MS acquisition. Samples were run twice, once under positive ESI‐MS/MS and once under negative ESI‐MS/MS to enable the identification of compounds that preferentially ionize with different polarities.ResultsGC analysis identified 0.64±0.05 μg of palmitic acid (C16:0) and 0.88±0.04 μg stearic acid (C18:0) per 6mm punch from 903 protein saver cards, 0.97±0.08 μg 16:0 and 1.43±0.16 μg 18:0 per 6mm punch of Whatman chromatography paper and 0.64±0.08 μg 16:0 and 0.88±0.10 μg 18:0 per Mitra tip. In the positive ESI‐MS/MS analyses, scanning for fragment losses of phospholipids (choline, ethanolamine, serine head groups) did not result in extracted ion chromatograms that would indicate that these compounds were present. Neutral‐loss scanning of fatty acids like palmitate and stearate in positive ESI also showed no evidence of other complex lipids such as triacylglycerols or cholesteryl esters in the blank samples. However, negative ESI‐MS/MS experiments confirmed that the palmitate and stearate that were identified using GC are found as free fatty acids and not as part of complex lipids.ConclusionsMaterials used to collect dried blood spots appear consistently contaminated with palmitic and stearic free fatty acids. GC determinations of fatty acids from dried blood spots samples need to consider this contamination and/or take steps to prewash sample collecting materials. For lipidomic analysis, these contaminants can be ignored if complex lipids and not free fatty acids are being examined.Support or Funding InformationThis work was supported by a Natural Sciences and Engineering Research Council (NSERC) Discovery grant (327149, to K.D.S), and an NSERC doctoral scholarship to J.J.A.H. K.D.S. is also supported by a Canada Research Chair in Nutritional Lipidomics.
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Hollender, Juliane, Emma L. Schymanski, Lutz Ahrens, Nikiforos Alygizakis, Frederic Béen, Lubertus Bijlsma, Andrea M. Brunner, et al. "NORMAN guidance on suspect and non-target screening in environmental monitoring." Environmental Sciences Europe 35, no. 1 (September 4, 2023). http://dx.doi.org/10.1186/s12302-023-00779-4.
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AbstractIncreasing production and use of chemicals and awareness of their impact on ecosystems and humans has led to large interest for broadening the knowledge on the chemical status of the environment and human health by suspect and non-target screening (NTS). To facilitate effective implementation of NTS in scientific, commercial and governmental laboratories, as well as acceptance by managers, regulators and risk assessors, more harmonisation in NTS is required. To address this, NORMAN Association members involved in NTS activities have prepared this guidance document, based on the current state of knowledge. The document is intended to provide guidance on performing high quality NTS studies and data interpretation while increasing awareness of the promise but also pitfalls and challenges associated with these techniques. Guidance is provided for all steps; from sampling and sample preparation to analysis by chromatography (liquid and gas—LC and GC) coupled via various ionisation techniques to high-resolution tandem mass spectrometry (HRMS/MS), through to data evaluation and reporting in the context of NTS. Although most experience within the NORMAN network still involves water analysis of polar compounds using LC–HRMS/MS, other matrices (sediment, soil, biota, dust, air) and instrumentation (GC, ion mobility) are covered, reflecting the rapid development and extension of the field. Due to the ongoing developments, the different questions addressed with NTS and manifold techniques in use, NORMAN members feel that no standard operation process can be provided at this stage. However, appropriate analytical methods, data processing techniques and databases commonly compiled in NTS workflows are introduced, their limitations are discussed and recommendations for different cases are provided. Proper quality assurance, quantification without reference standards and reporting results with clear confidence of identification assignment complete the guidance together with a glossary of definitions. The NORMAN community greatly supports the sharing of experiences and data via open science and hopes that this guideline supports this effort.