Article
Biochemical Research Methods
Monika Kijewska, Michalina Zawadzka, Karolina Wlodarczyk, Piotr Stefanowicz
Summary: The biomarker strategy based on specific glycation sites in plasma proteins can improve glycemic control and disease prediction. Glycated albumin, fibrinogen, and CD59 protein have been shown to be related to diabetes, and the level of glycation of individual lysine residues in proteins is crucial in disease progression. Quantification of new biomarkers requires isotope-labeled analogs for accurate data and detection of low-abundance biomarkers. The proposed synthesis method enables the study of glycated peptides.
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Organic
Brandon M. Young, Paolo Rossi, P. Jake Slavish, Yixin Cui, Munia Sowaileh, Jitendra Das, Charalampos G. Kalodimos, Zoran Rankovic
Summary: Isotopically labeled amino acids are commonly used for studying protein structure and dynamics by NMR. This study presents a facile gram-scale synthesis of compounds 1b and 2b under standard laboratory conditions from a common intermediate. The improved signal intensity with lower amounts of labeled precursor makes 1b and 2b potential alternatives to current labeling approaches.
Article
Chemistry, Multidisciplinary
Martin D. Gelenter, Ad Bax
Summary: Post-translational modifications are commonly found in eukaryotic proteomes. However, these modifications are rarely studied using NMR in eukaryotic proteins, which are usually produced in E. coli through recombinant expression. The native C-terminal amide of melittin, a major peptide in honey bee venom, significantly affects its structure and dynamics. This study presents a method to produce isotopically labeled native melittin through recombinant expression and chemical amidation. It also confirms the accuracy of structural models generated by AlphaFold-Multimer using experimental residual dipolar couplings.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2023)
Article
Chemistry, Applied
Sumei Ren, Mark A. Huffman, Aaron M. Whittaker, Hao Yang, Christopher C. Nawrat, David J. Waterhouse, Kevin M. Maloney, Neil A. Strotman
Summary: The synthesis of the carbon-14-labeled unnatural nucleoside islatravir, an investigational HIV drug, was achieved through a one-pot biocatalytic cascade starting from acetaldehyde-2-C-14. Combining enzymatic reactions into multistep biocatalytic cascades not only accelerates delivery and increases the yield, but also eliminates handling of radioactive intermediates and minimizes radioactive waste.
ORGANIC PROCESS RESEARCH & DEVELOPMENT
(2021)
Article
Chemistry, Analytical
Zhangjie Wang, Katelyn Arnold, Vijay M. Dhurandahare, Yongmei Xu, Vijayakanth Pagadala, Erick Labra, Walter Jeske, Jawed Fareed, Marla Gearing, Jian Liu
Summary: This study describes a LC-MS/MS-based method to analyze the structural motifs of 3-O-sulfated heparan sulfate (HS). The method was used to determine the levels of 3-O-sulfated HS in pharmaceutical heparin and human brain. The study found that a specific 3-O-sulfated structural motif, tetra-1, was elevated in the brain HS from Alzheimer's disease patients.
ANALYTICAL CHEMISTRY
(2022)
Article
Engineering, Environmental
Millaray Sierra-Olea, Simon Koelle, Emil Bein, Thorsten Reemtsma, Oliver J. Lechtenfeld, Uwe Huebner
Summary: As ozonation becomes a widespread treatment for removal of chemicals of emerging concern from wastewater treatment plant effluents, there are increasing concerns regarding the formation of ozonation products (OPs) and their potential impacts on the aquatic environment and human health. This study developed a new method using heavy oxygen (18O2) to label OPs from oxygen transfer reactions, and successfully confirmed the formation pathways of OPs from sulfameth-oxazole. The results provide insights into the mechanisms of ozonation and the potential to monitor and understand the formation of OPs in wastewater treatment processes.
Article
Chemistry, Analytical
Andrea Cerrato, Sara Elsa Aita, Anna Laura Capriotti, Chiara Cavaliere, Carmela Maria Montone, Susy Piovesana, Aldo Lagana
Summary: High-resolution mass spectrometry is a powerful tool for lipidomics analysis, especially for polar lipids such as glycerophospholipids and sphingolipids. In this study, a buffer modification workflow using labeled and unlabeled acetate ions was optimized and successfully applied to characterize phosphocholine-containing lipids in human plasma samples. This new workflow allows for accurate determination of lipid composition and molecular formulas, reducing false-positive rates and streamlining manual validation steps.
ANALYTICAL CHEMISTRY
(2021)
Article
Biochemistry & Molecular Biology
Buyan Pan, Joo Hyung Park, Trudy Ramlall, David Eliezer, Elizabeth Rhoades, E. James Petersson
Summary: This study explores the impact of post-translational modifications on alpha-synuclein and introduces a streamlined method to produce phosphorylated alpha S in large quantities. By co-expressing a kinase with a protein fragment in Escherichia coli and using methyl thioglycolate, the researchers achieved high yields of site-specifically phosphorylated protein through chemoenzymatic methods. This strategy is particularly suitable for producing N-15-labeled, phosphorylated protein for NMR studies.
Article
Agriculture, Multidisciplinary
Matthias Kasimir, Matthias Behrens, Hans-Ulrich Humpf
Summary: This study investigated whether lignin is metabolized by the gut microbiota using the ex vivo pig cecum model. Ten small phenolic lignin degradation products were identified and their quantity was estimated.
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
(2022)
Article
Chemistry, Organic
Shilong Zheng, Jiawang Liu, Borui Kang, Guangdi Wang
Summary: ZB716-d6, a deuterated form of ZB716, was successfully synthesized in eight steps from a commercially available deuterium-labeled starting material and has been utilized as an internal standard in clinical bioanalysis with good yield and high purity.
SYNTHETIC COMMUNICATIONS
(2022)
Article
Biochemistry & Molecular Biology
Cat Hoang Vesely, Patrick N. Reardon, Zhen Yu, Elisar Barbar, Ryan A. Mehl, Richard B. Cooley
Summary: Phosphoserine (pSer) sites are primarily located within disordered protein regions. Producing labeled proteins with site-specific pSer for NMR studies is important for understanding the molecular mechanisms of protein regulation. However, methodologies for adapting pSer genetic code expansion to minimal or isotope-enriched media have not been described.
JOURNAL OF BIOLOGICAL CHEMISTRY
(2022)
Article
Chemistry, Analytical
Cassio Lima, Howbeer Muhamadali, Yun Xu, Mustafa Kansiz, Royston Goodacre
Summary: This study demonstrates the use of infrared spectroscopy to track the uptake of stable isotope-labeled compounds by bacteria at the single-cell level, providing insights into microbial systems. The development of a new far-field infrared imaging technique, optical photothermal infrared (O-PTIR) spectroscopy, allows for monitoring the metabolic activity of individual bacteria and predicting isotopic ratios simultaneously using spectral signatures.
ANALYTICAL CHEMISTRY
(2021)
Article
Chemistry, Analytical
Emily Awuor Ouma, Helga Huszar, Laszlo Horvath, Gabor Szabo, Csaba Janaky, Zoltan Bozoki
Summary: In this work, a near-infrared diode laser-based photoacoustic system was used to achieve quasi-simultaneous measurement of 14NH3 and 15NH3 concentrations. By selecting appropriate wavelengths and using fast tuning methods, sensitive detection was achieved while avoiding interference.
ANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Organic
Eduardo Izquierdo, Marta L. opez-Corrales, Diego Abad-Montero, Anna Rovira, Gemma Fabria, Manel Bosch, Jose Luis Abad, Vicente Marchan
Summary: Researchers have developed a series of new fluorescent sphingolipid probes with excellent emission quantum yields and different subcellular localization patterns.
JOURNAL OF ORGANIC CHEMISTRY
(2022)
Article
Chemistry, Multidisciplinary
Seong-Joo Lee, Kwon Kyu Yu, Seong-min Hwang, Sangwon Oh, Nam Woong Song, Hak-Sung Jung, Oc Hee Han, Jeong Hyun Shim
Summary: Low-field nuclear magnetic resonance spectroscopy provides limited spectral information, but the use of isotopically labeled molecules can overcome this limitation. This study investigates the correlation spectroscopy of 1-C-13-ethanol at low-field, demonstrating that even with a moderate spectral line width, a low-field 2D spectrum can reveal the coupling networks of isotopically labeled molecules.
Article
Chemistry, Physical
Matthew P. Kroonblawd, Batikan Koroglu, Joseph M. Zaug, Philip F. Pagoria, Nir Goldman, Eran Greenberg, Vitali B. Prakapenka, Martin Kunz, Sorin Bastea, Elissaios Stavrou
JOURNAL OF CHEMICAL PHYSICS
(2018)
Article
Chemistry, Physical
David G. Weisz, Jonathan C. Crowhurst, Mikhail S. Finko, Timothy P. Rose, Batikan Koroglu, Reto Trappitsch, Harry B. Radousky, Wigbert J. Siekhaus, Michael R. Armstrong, Brett H. Isselhardt, Magdi Azer, Davide Curreli
JOURNAL OF PHYSICAL CHEMISTRY A
(2018)
Article
Physics, Fluids & Plasmas
Batikan Koroglu, Marco Mehl, Jonathan C. Crowhurst, Joseph M. Zaug, Timothy P. Rose, Harry B. Radousky, Michael R. Armstrong
PLASMA PHYSICS AND CONTROLLED FUSION
(2019)
Article
Chemistry, Analytical
Batikan Koroglu, Zurong Dai, Mikhail Finko, Michael R. Armstrong, Jonathan C. Crowhurst, Davide Curreli, David G. Weisz, Harry B. Radousky, Kim B. Knight, Timothy P. Rose
ANALYTICAL CHEMISTRY
(2020)
Article
Spectroscopy
Emily N. Weerakkody, David G. Weisz, Jonathan Crowhurst, Batikan Koroglu, Timothy Rose, Harry Radousky, Ryan L. Stillwell, Jason R. Jeffries, Nick G. Glumac
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
(2020)
Article
Chemistry, Applied
Batikan Koroglu, Jonathan C. Crowhurst, Evan M. Kahl, Jason S. Moore, Ana Racoveanu, Harris E. Mason, David G. Weisz, John G. Reynolds, Alan K. Burnham
Summary: This study presents real-time measurements of the product gases arising from the thermal decomposition of TATB and its derivatives, as well as LX-17, using IR absorption spectroscopy. The kinetics of deuterated TATB decomposition is slower than that of unsubstituted TATB due to the kinetic-isotope-effect, while the rate of LX-17 decomposition is slightly lower than unsubstituted TATB. The results suggest that the thermal decomposition mechanism of TATB may involve a series of pathways rather than a set of independent and parallel reactions.
PROPELLANTS EXPLOSIVES PYROTECHNICS
(2021)
Article
Chemistry, Applied
Keith R. Coffee, Adele F. Panasci-Nott, Benjamin J. Stewart, Jason A. Olivas, Audrey M. Williams, John G. Reynolds
Summary: This article reports a fast and sensitive method for determining the purity of TATB in polymer-bonded materials, and identifies the individual components using mass spectrometry and chromatography techniques. The accuracy and details of the method are reported.
PROPELLANTS EXPLOSIVES PYROTECHNICS
(2022)
Review
Spectroscopy
Elizabeth J. Kautz, Emily N. Weerakkody, Mikhail S. Finko, Davide Curreli, Batikan Koroglu, Timothy P. Rose, David G. Weisz, Jonathan C. Crowhurst, Harry B. Radousky, Michael DeMagistris, Neeraj Sinha, Deborah A. Levin, Ed L. Dreizin, Mark C. Phillips, Nick G. Glumac, Sivanandan S. Harilal
Summary: Studies on U gas-phase oxidation through plasma- and thermo-chemistry are crucial for various fields, using optical spectroscopy tools and computational modeling. The evolution from U atoms to U oxide molecules to nanoparticles and agglomerates is discussed in the context of optical spectroscopic studies.
SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
(2021)
Article
Construction & Building Technology
Maxwell A. T. Marple, Batikan Koroglu, Keith Morrison, Jonathan Crowhurst, Anagi Balachandra, Parviz Soroushian, Harris E. Mason
Summary: The combination of alkali-activation and mechanochemical milling in a CO2 rich atmosphere for synthesizing cementitious materials shows promise in upcycling hazardous materials and capturing CO2. Structural transformations during synthesis and hydration were studied using solid-state Al-27, Si-29, and C-13 NMR techniques.
CEMENT AND CONCRETE RESEARCH
(2022)
Article
Multidisciplinary Sciences
Mark A. Burton, Alex W. Auner, Jonathan C. Crowhurst, Peter S. Boone, Lauren A. Finney, David G. Weisz, Batikan Koroglu, Igor Jovanovic, Harry B. Radousky, Kim B. Knight
Summary: In this study, the influence of oxygen on rapidly cooling uranium was investigated through laser ablation of uranium metal in different concentrations of oxygen gas. The analysis of recovered particulates revealed that the micrometer-sized particulates are mainly amorphous UOx and UO2, and they convert to alpha-U3O8 when heated. It was also found that cooling timescales can affect the structural composition of uranium oxides.
SCIENTIFIC REPORTS
(2022)
Article
Chemistry, Multidisciplinary
Kate Rodriguez, Batikan Koroglu, Joshua Hammons, Zurong Dai, Maryline G. Ferrier, Enrica Balboni, Timothy Rose, Kim B. Knight
Summary: Local conditions like temperature and oxygen availability play a significant role in the formation and evolution of fallout following a nuclear explosion. This study focuses on the behavior of cerium oxide nanoparticles under controlled temperature and oxygen fugacities, finding that the gas-phase oxidation rate of cerium is influenced by temperature and local redox conditions. Post-condensation particle evolution is primarily driven by temperature, with particle size increasing as particles cool and aggregate.
ACS EARTH AND SPACE CHEMISTRY
(2022)
Article
Chemistry, Applied
Alan K. Burnham, Keith R. Coffee, Gregory L. Klunder, Adele F. Panasci-Nott, John G. Reynolds
Summary: The thermal degradation of TATB was analyzed using two small-scale analytical methods: simultaneous differential scanning calorimetry and thermogravimetric analysis (SDT), and a hot-stage microscope with Fourier Transform Infrared (FTIR) analysis capabilities. The results showed that TATB displayed a sigmoidal decrease in concentration during isothermal heating, while other soluble products increased and then abruptly declined in concentration. FTIR analysis revealed gradual changes in the amino and nitro functionality of TATB, and the extracted residues examined also showed a change in chemical composition between different treatment times. The establishment of a reliable mass- and energy-balanced global reaction network for TATB degradation requires the consideration of autocatalytic reactions with low activation energies.
PROPELLANTS EXPLOSIVES PYROTECHNICS
(2023)
Article
Chemistry, Applied
Keith R. Coffee, Adele F. Panasci-Nott, Jason A. Olivas, John Selinsky, Keith D. Morrison, Alan K. Burnham, Gregory L. Klunder, John G. Reynolds
Summary: Understanding the chemical composition and decomposition pathways of TATB residues produced from abnormal thermal environments is important. A methodology for isolating, identifying, and quantifying compounds in thermally treated TATB residues was reported. The study identified several trace compounds and proposed possible structures for unknown compounds.
PROPELLANTS EXPLOSIVES PYROTECHNICS
(2023)