Article
Chemistry, Analytical
Adilah Bahadoor, Andreas Brinkmann, Jeremy E. Melanson
Summary: Quantitative H-1 nuclear magnetic resonance (qHNMR) is an established method for determining purity in organic compounds, relying on careful selection of integrals and decoupling C-13 satellites to avoid interferences. Two decoupling schemes, GARP and bilevel adiabatic broadband decoupling, were explored, highlighting benefits and drawbacks of each. qH{C-13}NMR provides added clarity about the presence of impurities and tautomers, making it advantageous for accurate measurements compared to qHNMR.
ANALYTICAL CHEMISTRY
(2021)
Article
Chemistry, Multidisciplinary
Bryan S. Matsuura, Steven Huss, Zhaoxi Zheng, Shichen Yuan, Tao Wang, Bo Chen, John Badding, Dirk Trauner, Elizabeth Elacqua, Adri C. T. van Duin, Vincent H. Crespi, Klaus Schmidt-Rohr
Summary: The atomic-level structure of nanothreads produced by the slow compression of C-13(4)-furan was studied using advanced solid-state NMR. The majority of carbon atoms were found to be bonded to hydrogen, with a small percentage in different functional groups. The nanothreads exhibited both asymmetric and symmetric ring structures, with a portion of the carbon atoms forming highly ordered, fully saturated segments.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2021)
Article
Polymer Science
Johanna K. Elter, Jonas Eichhorn, Michael Ringleb, Felix H. Schacher
Summary: This study reports the synthesis and block copolymerization of three different glycidyl amines, leading to diblock terpolymers that can self-assemble into micelles with potential applications in drug delivery. These micelles exhibit pH-dependent disassembly or structural changes, as well as the ability to encapsulate and release hydrophobic small molecules under specific triggers.
Article
Food Science & Technology
Concetta Pironti, Maria Ricciardi, Oriana Motta, Federica Camin, Luana Bontempo, Antonio Proto
Summary: The study evaluated the feasibility of using C-13-NMR spectroscopy to determine the carbon stable isotope ratio of small organic molecules like vanillin, proving it to be a valuable alternative method. By comparing results from different analysis methods, the origin of vanillin can be accurately identified to ensure its quality.
Article
Chemistry, Multidisciplinary
Yu-Shan Wu, Bai-Xiang Li, Ying-Yun Long
Summary: This study aims to determine the conditions for high precision measurement of linear low density polyethylene (LLDPE). Nonuniform sampling (NUS) and band-selective HSQC are evaluated as time-saving strategies. The combination of band-selective HSQC and 50% NUS achieves significant precision enhancements and reduces experiment times.
Article
Chemistry, Multidisciplinary
Victor Ribay, Arnab Dey, Benoit Charrier, Clement Praud, Joris Mandral, Jean-Nicolas Dumez, Marine P. M. Letertre, Patrick Giraudeau
Summary: Hyperpolarized nuclear magnetic resonance (NMR) methods, particularly Dissolution Dynamic Nuclear Polarization (d-DNP), greatly enhance the sensitivity of detecting C-13 NMR signals. This study demonstrates the first application of d-DNP-enhanced C-13 NMR analysis of biofluid (urine) at natural abundance, providing unprecedented resolution and sensitivity. Accurate quantitative information on multiple targeted metabolites can be obtained through a standard addition procedure.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2023)
Article
Chemistry, Physical
Daphna Shimon, Kelly A. Cantwell, Linta Joseph, Ethan Q. Williams, Zaili Peng, Susumu Takahashi, Chandrasekhar Ramanathan
Summary: In this study, we achieved hyperpolarization of 13C nuclei in diamond at room temperature using microwave-induced dynamic nuclear polarization (DNP) technique, with enhancements of over 100-fold and improvement in signal averaging of the 1% abundant 13C spins by over 10,000-fold. Different enhancement features were observed for the central and outer nuclear spin manifolds, and frequency-chirped millimeter-wave excitation was found to improve the enhancements for the outer spin manifolds. The findings of this study have implications for spectroscopic studies with better chemical shift resolution at room temperature.
JOURNAL OF PHYSICAL CHEMISTRY C
(2022)
Article
Engineering, Chemical
Mohamed Gamal Mohamed, Ahmed M. Elewa, Meng-Syuan Li, Shiao-Wei Kuo
Summary: This study aimed to prepare Fe-Bi HPP and An-Bi HPP materials for I2 uptake and supercapacitors applications. The materials exhibited a narrow range of pore sizes and high specific surface area. The Fe-Bi HPP demonstrated superior efficiency in capturing iodine, with an impressive I2 adsorption uptake of 112.84 mg g-1.
JOURNAL OF THE TAIWAN INSTITUTE OF CHEMICAL ENGINEERS
(2023)
Article
Biochemistry & Molecular Biology
Pawel Siudem, Lukasz Szeleszczuk, Agnieszka Zielinska, Katarzyna Paradowska
Summary: Turmeric is a popular spice worldwide due to its anti-inflammatory properties attributed to curcumin. However, curcumin-containing dietary supplements face challenges of poor water solubility and synthetic curcumin substitution. This article proposes the use of C-13 CPMAS NMR method to analyze dietary supplements, and the results confirmed the presence of synthetic curcumin.
Article
Biochemical Research Methods
Marco Schiavina, Lorenzo Bracaglia, Maria Anna Rodella, Rainer Kuemmerle, Robert Konrat, Isabella Felli, Roberta Pierattelli
Summary: Nuclear magnetic resonance (NMR) spectroscopy is a powerful technique for characterizing biomolecules at atomic resolution. The availability of ultra-high-field NMR instrumentation has opened up new possibilities for studying more complex systems, such as flexible proteins and protein regions. While conducting experiments at such high field strengths comes with challenges, strategies and tricks can be employed to optimize the experiments.
Article
Thermodynamics
He Yang, Yankun Xiong, Zhouwei Xie, Lijun Jin, Yang Li, Juan Yang, Haoquan Hu
Summary: This paper proposes a method for quantitatively characterizing the carbon skeletal structure of coal using high-resolution CP/MAS 13C solid-state NMR spectroscopy, with Naomaohu coal as the experimental sample. The fractions of different carbons in coal were divided by analyzing the change of polarization transfer with contact time. The results obtained from this study are in agreement with previous literature and provide insight into the carbon structure of coal.
PROCEEDINGS OF THE COMBUSTION INSTITUTE
(2021)
Article
Polymer Science
Yasuhiro Kohsaka, Koki Nagai
Summary: Interfacial polymerization results in regulated monomer junctions and increased crystallinity of the resulting polymers, while terpolymerization with dicarboxylic acid chloride leads to controlled monomer sequences with uniformly distributed acrylate moieties, enhancing curability efficiency.
MACROMOLECULAR RAPID COMMUNICATIONS
(2021)
Article
Forestry
Sonoka Miyata, Dan Aoki, Yasuyuki Matsushita, Miyuki Takeuchi, Kazuhiko Fukushima
Summary: This study cultivated Ginkgo biloba L. saplings in a growth chamber with C-13 for two months. The C-13 ratio of the newly developed xylem region was evaluated using high lateral resolution secondary ion mass spectrometry and thioacidolysis/GC-MS. Solid-state C-13 direct polarisation/magic angle spinning (DP/MAS) NMR measurements were conducted for different wood samples, and the results suggested structural alterations of lignin during the sample preparation procedure, including ball milling.
Review
Chemistry, Multidisciplinary
Isabella C. Felli, Roberta Pierattelli
Summary: Modern C-13 NMR has become a valuable tool for biomolecular applications, allowing for complete assignment of proteins and providing unique information. A wide range of NMR observables can be measured to characterize the structure and dynamics of proteins comprehensively.
Article
Biochemistry & Molecular Biology
Yan Xue, Karolina Ucieklak, Suresh Gohil, Tomasz Niedziela, Gustav Nestor, Corine Sandstrom
Summary: This study presents a method of metabolic labeling of hyaluronan (HA) using Streptococcus equi subsp. Zooepidemicus and subsequent analysis by NMR and mass spectrometry. The results provide a valid approach for the quantitative assessment of isotopically labeled glycans and will enhance detection capabilities and facilitate structure-function relationship analysis of complex glycans.
CARBOHYDRATE RESEARCH
(2023)
Article
Chemistry, Multidisciplinary
Seong-Min Jo, Jihye Kim, Ji Eun Lee, Frederik R. Wurm, Katharina Landfester, Sanghyuk Wooh
Summary: This study investigates a novel multimodal enzyme- and photocatalyst-carrying superstructure for colorimetric glucose detection. By utilizing surface-templated evaporation driven suprastructure synthesis, superstructures comprising enzyme-carrying nanoparticles were successfully fabricated. The multimodal enzyme-carrying superstructures demonstrate promising potential for highly sensitive glucose detection in confined environments.
Article
Chemistry, Multidisciplinary
Seong-Min Jo, Hyeong Seok Kim, Miae Won, Carole Champanhac, Jong Seung Kim, Frederik R. Wurm, Katharina Landfester
Summary: The combination of nanoreactors and prodrugs presents great potential in anticancer treatment. However, the precise targeting of cancer cells remains a challenge. In this study, a dual-targeting approach using folate receptor-targeted nanoreactors and cyclooxygenase-2 (COX-2) targeted prodrugs is proposed. This strategy can generate synergistic effects and contribute to the development of selective and effective anticancer therapeutics.
ADVANCED FUNCTIONAL MATERIALS
(2022)
Article
Chemistry, Medicinal
Chiara Pelosi, Lorenzo Arrico, Francesco Zinna, Frederik R. Wurm, Lorenzo Di Bari, Maria R. Tine
Summary: Protein-polymer conjugates are a promising hybrid system with high biomedical potential. In this study, the thermal stability of a set of fully-degradable polyphosphoester-protein conjugates was evaluated using variable temperature circular dichroism. A simple and effective protocol was proposed to obtain useful information about these systems in vitro, which can be used for screening new samples in their early stages.
Article
Polymer Science
Shivani P. Wadgaonkar, Sandra Schuettner, Elena Berger-Nicoletti, Axel H. E. Mueller, Holger Frey
Summary: This study reports the synthesis and real-time 1H NMR kinetic studies on the living anionic copolymerization of 4-trimethylsilylstyrene (4TMSS). The results reveal an intriguing gradient microstructure in the synthesized copolymers, with 4TMSS exhibiting higher reactivity compared to styrene. Furthermore, the properties of the copolymers can be tailored by varying the content of 4TMSS.
Article
Engineering, Environmental
Stefan Peil, Hubert Gojzewski, Frederik R. Wurm
Summary: Bio-based and biodegradable cellulose acetals, with their reversible modification of cellulose, provide a versatile and sustainable alternative to non-degradable polyolefin plastics. These cellulose acetals are characterized by solubility in common organic solvents, adjustable physical properties, and the ability to undergo full degradation in compost and enzymatic processes. With the increasing urgency of climate change and plastic pollution, these cellulose derivatives offer a promising solution for a more sustainable future.
CHEMICAL ENGINEERING JOURNAL
(2023)
Review
Polymer Science
Zhong H. W. Easton, Mike A. J. Essink, Laura Rodriguez Comas, Frederik R. R. Wurm, Hubert Gojzewski
Summary: Biobased and biodegradable polymers are used in bioplastics to adjust their physical properties and biodegradation stability. Mixing with faster degrading polymers or fillers is a strategy to control degradation rates. This review focuses on representative examples of bioplastic blends and composites in applications such as tissue engineering, agriculture, or packaging, with a focus on accelerating biodegradation rates and preventing microplastic formation.
MACROMOLECULAR CHEMISTRY AND PHYSICS
(2023)
Article
Polymer Science
Timo Rheinberger, Mareike Deuker, Frederik R. Wurm
Summary: In this study, the degradation rate of polyphosphoesters (PPEs) with different side-chain structures under different pH conditions was investigated. The degradation mechanism was found to be influenced by the type and size of the side-chain and pH. By modifying the structure of the polyphosphonates or introducing additional breaking points, the half-life of the polymer could be tuned. This study highlights the versatile stability and controllability of water-soluble PPEs, making them promising for various applications, such as tissue regrowth.
EUROPEAN POLYMER JOURNAL
(2023)
Article
Polymer Science
Natkritta Huppe, Tassilo Gleede, Frederik R. Wurm
Summary: Poly(alkyl cyanoacrylate)s (PACAs) are widely used as adhesives in engineering and medicine. Achieving precise polymer structures is crucial, particularly for medical applications. By using a small amount (1%) of superbases to activate a functional thiophenol (PhSH) initiator, well-defined PACAs with adjustable molecular weights and moderate dispersities can be synthesized.
POLYMER INTERNATIONAL
(2023)
Article
Chemistry, Multidisciplinary
Yunbo Chen, Daniil Nozdriukhin, Sandra Michel-Souzy, Clemens Padberg, Frederik R. R. Wurm, Daniel Razansky, Xose Luis Dean-Ben, Olga Koshkina
Summary: Optoacoustic imaging combines optical contrast with ultrasound resolution in biological tissues. Inorganic particles have potential toxic effects, thus bio-based, biodegradable nano- and microcapsules with clinically-approved ICG are introduced. These capsules can enhance OA imaging and enable the localization and tracking of larger microcapsules.
Article
Polymer Science
Maria Brio Perez, Mark A. Hempenius, Sissi de Beer, Frederik R. Wurm
Summary: Polymer brushes are widely used for versatile surface modifications but most of them are nonbiodegradable. In this study, the researchers presented a synthetic strategy for grafting degradable polymer brushes via organocatalytic surface-initiated ring-opening polymerization. The polymer brushes produced were able to hydrolyze with controlled patterns and be regrown on the same substrate after degradation. The research showed that the polyester brush coatings exhibited different levels of hydrolytic stability and degradation mechanism, making them a potential alternative to nondegradable polymer brushes.
Article
Multidisciplinary Sciences
Olga Koshkina, Timo Rheinberger, Vera Flocke, Anton Windfelder, Pascal Bouvain, Naomi M. Hamelmann, Jos M. J. Paulusse, Hubert Gojzewski, Ulrich Floegel, Frederik R. Wurm
Summary: This study demonstrates the modification of biodegradable polyphosphoesters and tailoring the polymers' microstructure to adjust MRI relaxation times, addressing the issues of environmental pollution and organ accumulation caused by MRI agents. In vivo monitoring of polymers is crucial for drug delivery and tissue regeneration.
NATURE COMMUNICATIONS
(2023)
Article
Materials Science, Multidisciplinary
Tjerk R. Watt, Stefan Peil, Wendy A. Jonkers, Jurjen A. Regenspurg, Frederik R. Wurm, Wiebe M. de Vos
Summary: Polyelectrolyte multilayers (PEMMs) are versatile materials for nanofiltration membranes, but their nonrenewable nature raises sustainability concerns. This study proposes lignin as a renewable and biodegradable alternative for PEMM fabrication. Experimental results demonstrate that lignin can effectively replace fossil-based polyelectrolytes, producing PEMMs with excellent nanofiltration properties and stability.
ACS APPLIED POLYMER MATERIALS
(2023)
Article
Chemistry, Multidisciplinary
Diego A. Resendiz-Lara, Suna Azhdari, Hubert Gojzewski, Andre H. Groeschel, Frederik R. Wurm
Summary: In this work, water-soluble and degradable bottlebrush polymers were synthesized via ROMP using polyphosphoesters (PPEs) as the base material. PPE-macromonomers were first synthesized via organocatalytic anionic ring-opening polymerization and then used in ROMP to produce well-defined bottlebrush polymers. The resulting polymers showed good solubility in water and were degradable, making them promising for various biomedical applications.
Article
Chemistry, Physical
Natkritta Hueppe, Jenny Schunke, Michael Fichter, Volker Mailaender, Frederik R. Wurm, Katharina Landfester
Summary: Encapsulating multiple adjuvants and antigens into nanocarriers allows for synergistic induction of strong immune responses. A strategy to encapsulate a triple combination of adjuvants, including Resiquimod (R848), muramyl dipeptide (MDP), and polyinosinic-polycytidylic acid (Poly(I:C)), into human serum albumin (HSA) nanocarriers was developed. High encapsulation efficiency was achieved regardless of the physical properties of the cargoes, and the nanocarriers demonstrated efficient uptake and additive cell activation and maturation by dendritic cells.
NANOSCALE HORIZONS
(2022)
Article
Nanoscience & Nanotechnology
Chiara Pelosi, Iren Constantinescu, Helena H. Son, Maria Rosaria Tine, Jayachandran N. Kizhakkedathu, Frederik R. Wurm
Summary: This study evaluated the blood compatibility of water-soluble PPEs and PPE-coated model nanocarriers. The results showed that PPEs exhibited high hemocompatibility, with hydrophilic PPEs having no significant impact on blood coagulation, platelet activation, red blood cells lysis or aggregation. Even when a more hydrophobic copolymer was studied, changes in blood clot strength were only detected at high concentrations that are not typically used in biomedical applications.
ACS APPLIED BIO MATERIALS
(2022)
