Magnetic Resonance in Chemistry最新文献

Probing Spatial Proximities Between Protons of Collagen Protein in Native Bone Using 2D ¹H Multiple Quantum Experiments Under Fast MAS NMR.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2025-01-01 DOI: 10.1002/mrc.5508

Bijaylaxmi Patra, Vipin Agarwal, Yusuke Nishiyama, Neeraj Sinha

{"title":"Probing Spatial Proximities Between Protons of Collagen Protein in Native Bone Using 2D 1H Multiple Quantum Experiments Under Fast MAS NMR.","authors":"Bijaylaxmi Patra, Vipin Agarwal, Yusuke Nishiyama, Neeraj Sinha","doi":"10.1002/mrc.5508","DOIUrl":"https://doi.org/10.1002/mrc.5508","url":null,"abstract":"In solid-state nuclear magnetic resonance (ssNMR) spectroscopy, fast magic angle spinning (MAS) is a potent technique that efficiently reduces line broadening and makes it possible to probe structural details of biological systems in high resolution. However, its utilization in studying complex heterogeneous biomaterials such as bone in their native state has been limited. The present study has demonstrated the feasibility of acquiring two-dimensional (2D) 1H-1H correlation spectra for native bone using multiple-quantum/single-quantum correlation experiments (MQ/SQ) at fast MAS (70 kHz). This method uncovered distinct 1H-1H dipolar coupling networks involving long-chain charged residues of collagen protein, highlighting their role in maintaining the stability of the collagen triple helix. Our study opens up new avenues for 1H-detected multi-quantum-based experiments at fast MAS on native collagen-containing biological systems to explore their complex heterogeneous structural details more efficiently.","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142915475","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Experimental and Computational NMR Studies of Large Alkaloids Exemplified With Vindoline Trimer: Advantages and Limitations.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2025-01-01 DOI: 10.1002/mrc.5502

Valentin A Semenov, Sergey V Zinchenko, Georges Massiot, Leonid B Krivdin

引用次数: 0

NMR Spectroscopic Reference Data of Synthetic Cannabinoids Sold on the Internet.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2025-01-01 DOI: 10.1002/mrc.5498

Eva-Maria Hubner, Martin G Schmid, Verina Manojlovic, Daniela Gattringer, Eva-Maria Pferschy-Wenzig, Olaf Kunert

{"title":"NMR Spectroscopic Reference Data of Synthetic Cannabinoids Sold on the Internet.","authors":"Eva-Maria Hubner, Martin G Schmid, Verina Manojlovic, Daniela Gattringer, Eva-Maria Pferschy-Wenzig, Olaf Kunert","doi":"10.1002/mrc.5498","DOIUrl":"https://doi.org/10.1002/mrc.5498","url":null,"abstract":"Besides classic illegal drugs, numerous designer drugs, also called new psychoactive substances (NPSs), are available on the global drug market. One of the biggest and fastest-growing substance classes comprises the synthetic cannabinoids. According to the European Monitoring Centre for Drugs and Drug Addiction (EMCDDA), 254 out of 950 monitored substances belong to this group of NPS, with 9 new cannabinoids registered for the first time in 2023. For their purchase, it is not necessary to use the dark web. Due to the structural differences compared to the illegal Δ9-THC (delta-9-tetrahydrocannabinol), the legal status changes and the synthetic cannabinoids are available via clear web pages. They come as powders or dissolved and sprayed onto non-psychoactive layers such as cannabidiol hemp, industrial hemp or also on other plant material like herbal tea mixtures or dried flowers. These adulterated plant parts can be smoked as a substitute to the psychoactive and in many countries illegal Δ9-THC-containing hemp. The main task of this project was to check the identity of online available synthetic cannabinoid samples and to generate experimental data using a combination of gas and liquid chromatography with mass spectrometric detection and NMR-based structure elucidation. In total, 25 substances in solid state were bought from various online shops. They turned out to be 21 synthetic cannabinoids after analysis, including 13 with no or incomplete experimental NMR data available in the literature and one, CH-PIATA, which has not been mentioned in literature yet. More than 50% of the acquired substances were falsely declared.","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142915473","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

DFT Calculations of ¹H and ¹³C NMR Chemical Shifts of Hydroxy Secondary Oxidation Products of Geometric Isomers of Conjugated Linoleic Acid Methyl Esters: Structures in Solution and Revision of NMR Assignments.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-26 DOI: 10.1002/mrc.5506

Themistoklis Venianakis, Michael G Siskos, Ioannis P Gerothanassis

{"title":"DFT Calculations of 1H and 13C NMR Chemical Shifts of Hydroxy Secondary Oxidation Products of Geometric Isomers of Conjugated Linoleic Acid Methyl Esters: Structures in Solution and Revision of NMR Assignments.","authors":"Themistoklis Venianakis, Michael G Siskos, Ioannis P Gerothanassis","doi":"10.1002/mrc.5506","DOIUrl":"https://doi.org/10.1002/mrc.5506","url":null,"abstract":"Detailed DFT studies of 1H and 13C NMR chemical shifts of hydroxy secondary oxidation products of various geometric isomers of conjugated linolenic acids methyl esters are presented. Several low energy conformers were identified for model compounds of the central dienenol OH moiety, which were found to be practically independent on the various functionals and basis sets used. This greatly facilitated the minimization process of the geometric isomers of conjugated linolenic acids methyl esters. Several regularities of the literature experimental 1H and 13C chemical shifts were reproduced very accurately with the computational chemical shifts of the Gibbs low energy DFT optimized conformers, after a Boltzmann analysis. δ(13C) and δ(1H) of the methine CH-OH group are highly diagnostic for the trans/trans and cis/trans geometric isomerism of the adjacent double bond. δ(13C) of the -CH2- group adjacent to the terminal double bond of the conjugated system strongly depend on the cis/trans geometric isomerism of this bond and, thus, could be of importance in structural analysis. Ambiguities in the reported literature resonance assignments of olefinic carbons had been resolved. Computational δ(1H) and δ(13C) can be utilized for the identification of geometric isomerism and structural and conformational elucidation of hydroxy derivatives of conjugated linoleic acids and their ester derivatives.","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2024-12-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142895749","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Computational NMR Structural Revision of Marinoaziridines A and B.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-20 DOI: 10.1002/mrc.5505

Armando Navarro-Vázquez

引用次数: 0

Cross-Correlation Between ¹¹B Quadrupole and ¹¹B-¹⁹F Dipole-Dipole Coupling in BF₂ Groups.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-20 DOI: 10.1002/mrc.5507

Franziska Rüttger, Dominik Franke, Jannik Probst, Xiaobai Wang, Dietmar Stalke, Michael John

引用次数: 0

Unlocking the Chemical Diversity of Plant Catharanthus roseus: Nuclear Magnetic Resonance Spectroscopy Approach.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-19 DOI: 10.1002/mrc.5504

Upasna Gupta, M P Kavya, K Jayalakshmi, Neeraj Sinha

{"title":"Unlocking the Chemical Diversity of Plant Catharanthus roseus: Nuclear Magnetic Resonance Spectroscopy Approach.","authors":"Upasna Gupta, M P Kavya, K Jayalakshmi, Neeraj Sinha","doi":"10.1002/mrc.5504","DOIUrl":"https://doi.org/10.1002/mrc.5504","url":null,"abstract":"Catharanthus roseus, also known as Madagascar periwinkle, is a perennial plant renowned for its extensive pharmacological properties. It produces vital chemotherapeutic compounds, including vinblastine and vincristine, and exhibits anti-inflammatory, antidiabetic, and antioxidant activities. In this study, we utilized a range of two-dimensional (2D) nuclear magnetic resonance (NMR) techniques, such as 1H-1H correlation spectroscopy (COSY), 1H-1H J-resolved NMR, and 1H-13C heteronuclear single quantum coherence (HSQC) sensitivity-enhanced NMR spectroscopy, to identify key metabolites in C. roseus leaf extracts. Given the presence of numerous metabolites with closely spaced multiplet resonances, the 1H NMR spectra often exhibit significant signal overlap, making metabolite identification difficult or even impossible. However, the use of 2D NMR techniques effectively overcame this challenge, allowing for the precise identification of important alkaloids, such as vindoline, vinblastine, serpentine, and ajmalicine, along with essential metabolites like organic acids, amino acids, and carbohydrates. The extract contained a variety of bioactive compounds, including organic acids crucial for the tricarboxylic acid (TCA) cycle, branched-chain amino acids vital for metabolic functions, and alkaloids with substantial therapeutic potential. This comprehensive study underscores the continued significance of C. roseus in both traditional and modern medicine, emphasizing its intricate metabolic network and its potential in the development of novel therapeutics.","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2024-12-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142864328","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Nuclear Magnetic Resonance Spectroscopic Characterization and Determination of the New Psychoactive Substance Benzylone: Application in a Biological Fluid.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-09 DOI: 10.1002/mrc.5500

D Florou, V A Boumba, G C Tsiafoulis

{"title":"Nuclear Magnetic Resonance Spectroscopic Characterization and Determination of the New Psychoactive Substance Benzylone: Application in a Biological Fluid.","authors":"D Florou, V A Boumba, G C Tsiafoulis","doi":"10.1002/mrc.5500","DOIUrl":"https://doi.org/10.1002/mrc.5500","url":null,"abstract":"New psychoactive substances (NPS)-designed to mimic various legal or illegal substances-are an emerging worldwide health problem. Their identification and quantification in either complex seized samples or powders are critical; moreover, their determination in biological fluids is an intriguing goal in the forensic toxicology field. Synthetic cathinones are one of the most important groups among NPS. The current paper was designed as a pilot study to investigate the application of NMR techniques to identify and quantify unknown NPS compounds in deuterated dimethyl sulfoxide (DMSO-d6) and in urine using the synthetic cathinone benzylone (3,4-methylenedioxy-N-benzylcathinone, BMDP) as a pilot compound. In the first part of our study, nuclear magnetic resonance (NMR) spectroscopic characterization was performed using 1D and 2D homonuclear and heteronuclear NMR spectroscopic methods as long as diffusion ordered spectroscopy (DOSY). Following the above, the assignment of benzylone in DMSO-d6 was performed, and a distinct spectroscopic pattern was proposed. In the second part of our study, a NMR spectroscopic approach was applied for benzylone identification and quantification in a spiked with benzylone urine. Following the above, the assignment of benzylone in spiked urine was performed. A distinct pattern of the H11, H14, H15, and H8 signals on the 1H NMR spectra was observed and suggested as a \"NMR spectroscopic pattern/signature\" enabling the identification of benzylone moieties in urine. On the other hand, the applied NMR techniques showed low sensitivity in quantitating benzylone in spiked urine. Overall, our results are promising in using NMR for structure determination of unknown compounds in urine.","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2024-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142801454","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Evaluation of Automatic Analysis Software for ¹H NMR Spectra Quantification. Impact of Signal Broadening and EDTA Addition.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-08 DOI: 10.1002/mrc.5503

Circe C Hernández-Espino, Martha E García-Aguilera, Alan Emmanuel Aguilar Valeriano, Nuria Esturau-Escofet

{"title":"Evaluation of Automatic Analysis Software for 1H NMR Spectra Quantification. Impact of Signal Broadening and EDTA Addition.","authors":"Circe C Hernández-Espino, Martha E García-Aguilera, Alan Emmanuel Aguilar Valeriano, Nuria Esturau-Escofet","doi":"10.1002/mrc.5503","DOIUrl":"https://doi.org/10.1002/mrc.5503","url":null,"abstract":"NMR is a well-established analytical technique that enables the identification and quantification of several compounds in complex mixtures. The implementation of automated analysis software enhances this process by comparing sample spectra with a library of standard reference spectra. One of the key parameters in libraries is the signal line width; however, this may result in a concentration bias for compounds with broad signals, particularly those that are complexing. This study aims to evaluate the quantification of seven compounds commonly present in wine with complexing activity. Four automatic programs and manual deconvolution were used to quantify mixtures of these compounds at known concentrations, both in the presence of cations and with the addition of ethylenediamine-tetraacetate (EDTA) as a chelating agent. Additionally, malate was quantified in a wine sample using the standard addition method, both with and without EDTA. The findings illustrate that three of the programs, which employ the signal width value, underestimate compound concentrations in the presence of cations due to signal broadening. This error was mitigated by the EDTA addition. In contrast, the remaining software, which did not utilize signal line width, obtained similar concentrations in both cases. Future investigations involving the automatic analysis of compounds with complexing activity should take care of sample preparation and/or algorithm selection. Furthermore, future software development should consider allowing flexible adjustments of signal line width in their workflow.","PeriodicalId":18142,"journal":{"name":"Magnetic Resonance in Chemistry","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2024-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142794959","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Structure Elucidation of New Kavalactone Dimers From Alpinia zerumbet Pericarps Using NMR Calculations.

IF 1.9 3区化学

Magnetic Resonance in Chemistry Pub Date : 2024-12-05 DOI: 10.1002/mrc.5501

Yuto Nishidono, Ken Tanaka

引用次数: 0