Article
Chemistry, Physical
Alexey S. Kiryutin, Ivan V. Zhukov, Fabien Ferrage, Geoffrey Bodenhausen, Alexandra V. Yurkovskaya, Konstantin L. Ivanov
Summary: ZULF-TOCSY is a novel nuclear magnetic resonance method that achieves correlations between different nuclei by evenly distributing polarization, allowing for sequential assignments in peptides and other samples with natural isotopic abundance. This method provides a valuable alternative to traditional 2D experiments, such as HMBC, by offering more comprehensive spectral information.
PHYSICAL CHEMISTRY CHEMICAL PHYSICS
(2021)
Article
Chemistry, Physical
Ivan Hung, Zhehong Gan, Gang Wu
Summary: This study presents two- and three-dimensional C-13-O-17 heteronuclear correlation solid-state NMR experiments under magic-angle spinning (MAS) conditions. The experiments were performed on different samples using various schemes to achieve coherence transfer between C-13 and O-17 nuclei. This new 3D O-17 NMR experiment aims for site-resolved solid-state O-17 NMR studies, demonstrating successful correlations between O-17, C-13, and C-13 nuclei.
JOURNAL OF PHYSICAL CHEMISTRY LETTERS
(2021)
Article
Energy & Fuels
Stef Ghysels, Jan Verwaeren, Hero Jan Heeres, Leon Rohrbach, Simon Backx, Sven Mangelinckx, Frederik Ronsse
Summary: Pyrolysis liquids are difficult to analyze comprehensively due to their complex and heterogeneous composition. The use of two-dimensional 1H-13C heteronuclear single-quantum correlation (HSQC) nuclear magnetic resonance (NMR) has gained renewed interest for quantitative recording, providing a valuable tool for fingerprinting and assessing these complex liquids. However, data analysis of 1H-13C HSQC spectra has been lacking behind recent experimental developments. This study explores and demonstrates a new approach for automated data analysis from 1H-13C HSQC spectra using image processing tools.
Article
Energy & Fuels
Stef Ghysels, Jan Verwaeren, Hero Jan Heeres, Leon Rohrbach, Simon Backx, Sven Mangelinckx, Frederik Ronsse
Summary: This article explores the use of image processing tools for automatic analysis of H-1-C-13 HSQC spectra, demonstrating its effectiveness.
Article
Chemistry, Physical
Andrea Simion, Tobias Schubeis, Tanguy Le Marchand, Mihai Vasilescu, Guido Pintacuda, Anne Lesage, Claudiu Filip
Summary: A new heteronuclear decoupling pulse sequence called ROSPAC is introduced, which enhances decoupling efficiency by using a large pattern of radio-frequencies and minimizing cross-effects. ROSPAC performs well for a wide range of chemical shifts and low radio-frequency powers, making it suitable for ultra-fast magic-angle spinning (MAS) conditions.
JOURNAL OF CHEMICAL PHYSICS
(2022)
Article
Chemistry, Organic
Daisuke Unabara, Masaki Nishijima
Summary: This Note describes the successful structural assignment of a proton-deficient nucleic acid analogue using the LR-HSQMBC technique, which is a 2D NMR method for detecting weak C-H spin couplings. Azathioprine, an immunosuppressant drug, was used as the target compound. The LR-HSQMBC measurements revealed the presence of covalent bonds between the purine and imidazole rings with good sensitivity.
JOURNAL OF ORGANIC CHEMISTRY
(2022)
Article
Chemistry, Organic
Daisuke Unabara, Masaki Nishijima
Summary: This Note describes the successful structural assignment of a proton-deficient nucleic acid analogue using the 1H-13C longrange heteronuclear single quantum multiple bond correlation (LRHSQMBC) technique. LR-HSQMBC is a 2D NMR technique for the sensitive detection of weak C-H spin couplings. The immunosuppressant drug, azathioprine, was used as the target compound, and the LR-HSQMBC measurements revealed covalent bonds between the purine and imidazole rings with good sensitivity.
JOURNAL OF ORGANIC CHEMISTRY
(2023)
Article
Environmental Sciences
Chen Xu, Peng Lin, Ravindranath Garimella, Dien Li, Wei Xing, Nicole E. Patterson, Daniel Kaplan, Chris M. Yeager, Patrick G. Hatcher, Peter H. Santschi
Summary: The complex behavior of iodine isotopes and their interaction with natural organic matter pose a challenge for transport models. This study investigates the iodination of humic and fulvic acid and shows how it chemically alters the behavior of these organic matter, potentially affecting their mobility in the environment.
SCIENCE OF THE TOTAL ENVIRONMENT
(2022)
Article
Chemistry, Multidisciplinary
Jin Wook Cha, Min-Seon Kim, Jin-Soo Park
Summary: The GEMSTONE method selectively excites a specific proton signal among complex NMR signals, but its extension to heteronuclear spin systems was unsuccessful. This study presents an extension method that addresses the polarization transfer efficiency issue in heteronuclear systems, enabling the acquisition of ultraselective C-13 and H-1-C-13 correlation NMR subspectra. The technique is demonstrated to be effective in the structural analysis of a chromopeptide pharmaceutical and a diastereomeric mixture of a fungicide.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2023)
Article
Chemistry, Inorganic & Nuclear
Sara A. Maute, Alexander A. Marchione, Elizabeth L. Diaz
Summary: The popular multiplicity-edited heteronuclear single quantum coherence experiment has been modified for 19F-13C experiments by inserting broadband inversion and refocusing pulses in 19F. This modification allows for distinguishing CF3 from CF2X and CF2 from CFX (X = O or halide). The experiment results show that phase distortions can be minimized by carefully selecting the value of JCF, and analogous editing can be performed by phase.
JOURNAL OF FLUORINE CHEMISTRY
(2023)
Article
Chemistry, Analytical
Joshua W. Peterson, Scott R. Burt, Yu Yuan, James K. Harper
Summary: Nuclear magnetic resonance (NMR) studies involving O-17 are becoming increasingly important, but the high cost of (H2O)-O-17 limits its use. A recent study proposed a low-cost distillation scheme to produce large quantities of (H2O)-O-17. This article describes an alternative reaction scheme to measure O-17 water, which is fast, produces only one O-17 product, and requires no cleanup step. The accuracy of the C-13 NMR analysis is high and accessible to most NMR spectroscopists.
ANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Inorganic & Nuclear
Joshua J. Woods, Jesse A. Spivey, Justin J. Wilson
Summary: The synthesis and characterization of the N-15-labeled analogue of the mitochondrial calcium uptake inhibitor Ru265 was reported. The reactivity of Ru265 towards biologically relevant small molecules was assessed, revealing its ability to form coordination bonds. Time-based studies suggest that hydrogen-bonding interactions may play a more significant role in mediating the inhibitory properties of this complex.
EUROPEAN JOURNAL OF INORGANIC CHEMISTRY
(2022)
Article
Chemistry, Physical
Rick W. Dorn, Alexander L. Paterson, Ivan Hung, Peter L. Gor'kov, Austin J. Thompson, Aaron D. Sadow, Zhehong Gan, Aaron J. Rossini
Summary: This study investigated pulse sequences for magic-angle spinning solid-state NMR experiments to probe the vicinity of quadrupolar spins. The experiments and numerical simulations allowed estimation of isotopic enrichment. Moreover, the practical application of these heteronuclear correlation experiments in probing structural connectivity between two quadrupolar spins was demonstrated.
JOURNAL OF PHYSICAL CHEMISTRY C
(2022)
Article
Chemistry, Physical
Tamar Wolf, Michael J. Jaroszewicz, Lucio Frydman
Summary: This study explores the use of two-dimensional QUadrupolar Isotope Correlation SpectroscopY (QUICSY) experiments to increase the NMR spectral resolution and enrich the characterization of quadrupolar NMR patterns under static conditions. The possibility of obtaining sharp ridges in 2D correlations for two quadrupolar isotopes of the same element is investigated, even in static samples showing large quadrupolar effects. The approach shows promising results in characterizing wide-line NMR spectra of quadrupolar nuclei with different nuclear isotopes.
JOURNAL OF PHYSICAL CHEMISTRY C
(2022)
Article
Biochemical Research Methods
Lenny Haddad, Sophie Renou, Gerald S. Remaud, Toufic Rizk, Joseph Bejjani, Serge Akoka
Summary: A high-precision NMR method for analyzing small quantities of cholesterol was developed in this study, which significantly reduces acquisition time through adiabatic pulses, optimized strategies, and adjusted parameters, enabling isotope analysis of matrices low in cholesterol.
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
(2021)
Article
Chemistry, Multidisciplinary
Davy Sinnaeve, Julian Ilgen, Maria Enrica Di Pietro, Johann J. Primozic, Volker Schmidts, Christina M. Thiele, Burkhard Luy
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2020)
Article
Biochemistry & Molecular Biology
Claudia Muhle-Goll, Philipp Eisenmann, Burkhard Luy, Stefan Koelker, Burkhard Toenshoff, Alexander Fichtner, Jens H. Westhoff
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
(2020)
Article
Chemistry, Multidisciplinary
Maria Enrica Di Pietro, Pavleta Tzvetkova, Thomas Gloge, Ulrich Sternberg, Burkhard Luy
Article
Chemistry, Multidisciplinary
Andreas Lingel, Anna Vulpetti, Tony Reinsperger, Andrew Proudfoot, Regis Denay, Alexandra Frommlet, Christelle Henry, Ulrich Hommel, Alvar D. Gossert, Burkhard Luy, Andreas O. Frank
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2020)
Article
Chemistry, Organic
Sebastian T. Jung, Luis Basche, Tony Reinsperger, Burkhard Luy, Joachim Podlech
EUROPEAN JOURNAL OF ORGANIC CHEMISTRY
(2020)
Article
Chemistry, Analytical
Andrea Bodor, Jens D. Haller, Chafiaa Bouguechtouli, Francois-Xavier Theillet, Laszlo Nyitray, Burkhard Luy
ANALYTICAL CHEMISTRY
(2020)
Article
Chemistry, Organic
Sebastian T. Jung, Roman Nickisch, Tony Reinsperger, Burkhard Luy, Joachim Podlech
Summary: The study investigated stereoelectronic effects in cyclohexanones and related compounds through coupling constant measurements and identification of Perlin effects. It was found that coupling constants are influenced by various factors, including stereoelectronic interactions and the s character of carbon orbitals. Reliable correlations between measured and calculated coupling constants were achieved using specific functionals.
JOURNAL OF PHYSICAL ORGANIC CHEMISTRY
(2021)
Article
Chemistry, Analytical
Tamas Gyongyosi, Istvan Timari, Davy Sinnaeve, Burkhard Luy, Katalin E. Kover
Summary: The article introduces the important step of resonance assignment in nuclear magnetic resonance analysis, as well as a new method combining HSQC and COSY experiments for faster structure elucidation.
ANALYTICAL CHEMISTRY
(2021)
Article
Chemistry, Multidisciplinary
Fanni Sebak, Peter Ecsedi, Wolfgang Bermel, Burkhard Luy, Laszlo Nyitray, Andrea Bodor
Summary: This study introduces two new NMR experiments to identify proline cis/trans isomers in proteins, detecting minor conformers present in 4-15%, and analyzes the impact of CK2 phosphorylation on the cis/trans-proline equilibrium. Statistical analysis indicates that the amino acid type also affects the distribution of cis/trans-proline.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2022)
Article
Biochemical Research Methods
Sebastian Ehni, Martin R. M. Koos, Tony Reinsperger, Jens D. Haller, David L. Goodwin, Burkhard Luy
Summary: This study presents a new method to improve refocusing performance by incorporating coupling evolution into pulse design. By optimizing the refocusing pulses, heteronuclear coherence transfer in delay pulse-delay-type sequences is achieved. Additionally, efficient J-compensated refocusing pulse sandwiches are optimized.
JOURNAL OF MAGNETIC RESONANCE
(2022)
Article
Biochemistry & Molecular Biology
Stella Slad, Wolfgang Bermel, Rainer Kummerle, Daniel Mathieu, Burkhard Luy
Summary: Biomolecular NMR spectroscopy requires high magnetic field strengths for high spectral resolution. This study presents band-selective universal rotation pulses with a higher ratio of selective bandwidth to maximum rf-amplitude, which perform better than standard pulses according to simulations.
JOURNAL OF BIOMOLECULAR NMR
(2022)
Article
Biochemistry & Molecular Biology
Jens D. Haller, Andrea Bodor, Burkhard Luy
Summary: We present a real-time pure shift acquisition scheme for the detection of amide protons, which can effectively suppress the full homo- and heteronuclear coupling network, leading to improved resolution and sensitivity.
JOURNAL OF BIOMOLECULAR NMR
(2022)
Article
Chemistry, Physical
Desiree Steuernagel, David Rombach, Daniel Sack, Martin Koos, Burkhard Luy, Hans-Achim Wagenknecht
Summary: A new method was developed to activate CCl3F using photoredox catalysis and functionalize alkenes with the CCl2F group. N-phenylphenothiazine was used as a highly reducing organophotocatalyst. This approach combines the efficient disposal of ozone depleting substances and greenhouse gases with the synthesis of valuable organic compounds, complements the concept of atom transfer radical addition, and provides direct synthetic access to the CCl2F group as a structural motif. The broad substrate scope and multifunctionalized product class enable various subsequent transformations.
Article
Chemistry, Organic
Fabian Hoffmann, Anna-Lena Leistner, Susanne Kirchner, Burkhard Luy, Claudia Muhle-Goll, Zbigniew Pianowski
Summary: This study presents a structural analysis of peptide-derived photochromic supramolecular hydrogels using advanced techniques of nuclear magnetic resonance. The hydrogels were physically loaded with a selection of biologically related compounds. The results provide detailed and correct understanding of the loading process and will guide the correct design of phototriggered drug delivery systems.
EUROPEAN JOURNAL OF ORGANIC CHEMISTRY
(2023)
Article
Physics, Multidisciplinary
David L. Goodwin, Martin R. M. Koos, Burkhard Luy
PHYSICAL REVIEW RESEARCH
(2020)
