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Signal amplification by reversible exchange (SABRE) employs the non-equilibrium spin order of parahydrogen as a source of strong nuclear magnetic resonance (NMR) signal enhancement, with the objective of increasing NMR sensitivity. In SABRE, a parahydrogen molecule and a substrate form a transient polarization transfer complex. Performed within the high magnetic field of an NMR spectrometer, SABRE enables the hyperpolarization of nuclear spins without additional polarizers. Nevertheless, it requires thorough pulse sequence design. The high-field polarization transfer strategy strongly depends on the type of the spin system formed by the parahydrogen-nascent protons in the SABRE complex: chemically equivalent or non-equivalent. SABRE hyperpolarization in chemically equivalent spin systems has been the subject of considerable attention, even after being relevant only for a limited number of substrates. Efficient hyperpolarization in chemically non-equivalent complexes remained a key challenge, hindering the full potential of high-field SABRE and the ability to polarize a broader range of SABRE substrates. This work reports the multinuclear 1H–15N pulse sequence for efficient 15N hyperpolarization in chemically non-equivalent SABRE complexes. This approach relies on the simultaneous 1H and 15N radiofrequency excitation of the complex-bound nuclei with weak continuous wave magnetic fields. The proposed pulse sequence enabled the hyperpolarization of the 15N nuclei in a mixture of the antimicrobial drugs containing a 5-nitroimidazol moiety at their natural 15N isotopic abundance (0.76% of 15N polarization). Furthermore, it permitted the precise assignment of the SABRE complexes responsible for the polarization transfer. [ABSTRACT FROM AUTHOR]

The determination of molar masses and their distributions is crucial in polymer synthesis and design. This work presents the current performance and limitations of diffusion‐ordered spectroscopy (DOSY) on a low‐field (benchtop) NMR spectrometer (at 90 MHz) as an alternative to size exclusion chromatography (SEC) for determining diffusion coefficient distributions (DCDs) and molar mass distributions (MMDs). After optimization for narrowly distributed homopolymers, MMDs obtained with inverse Laplace transformation (ILT) and log‐normal distribution are compared with average molar masses obtained with mono‐ and bi‐exponential fits, as well as MMDs obtained from SEC. This approach enables ILT to determine DCDs and MMDs even for bimodal homopolymers with fully spectrally overlapping signals and block copolymers with various chemical compositions, for which chemical composition profiles are determined. The feasibility of low‐field diffusion NMR with samples dissolved in non‐deuterated solvents is further demonstrated and methods for solvent suppression are discussed. [ABSTRACT FROM AUTHOR]

The exploitation of efficient lubricants for ABS resins is widely recognized as beneficial for industrial production. Fatty diamides are typically applied as the lubricants for ABS resins; however, the connection between fatty chain structures and the lubricating properties is still vague. In this work, a range of ethylenediamine‐based amide lubricants (EDA‐Cn) with different fatty chain structures were successfully prepared and chemical structures were characterized in detail by the Fourier transform infrared spectrometer and proton nuclear magnetic resonance. The rheological test results suggested that the complex viscosity and relaxation time were positively associated with the fatty chain lengths of EDA‐Cn. The dynamic mechanical analysis results confirmed that EDA‐Cn exhibited excellent compatibility with ABS resins. The lubricating effect of EDA‐Cn decreased with increasing fatty chain lengths, which was manifested by a higher glass transition temperature, and lower elongation at break of ABS resins. In comparison to EDA‐C22, the complex viscosity (angular frequency = 0.1 rad/s) and glass transition temperature of EDA‐C10 have decreased by 24.9% and 3.9%, respectively. The molecular dynamics simulations revealed the intrinsic mechanism of lubricant‐substrate interaction. The EDA‐Cn containing short fatty chain lengths reduced the interaction energy with the matrix, thereby promoting the diffusive movement of the chain segments, and resulted in the increase in the mean square displacement and improved flow properties. These findings provided sufficient theoretical basis for the rational design and preparation of lubricants for ABS resins. [ABSTRACT FROM AUTHOR]

Signal Amplification By Reversible Exchange (SABRE) can provide strong signal enhancement (SE) to an array of molecules through reversible exchange of parahydrogen (pH2) derived hydrides and a suitable substrate coordinated to a transition metal. Among the substrates that can be used as a probe for hyperpolarised NMR and MRI, pyruvate has gained much attention. SABRE can hyperpolarise pyruvate in a low cost, fast, and reversible fashion that does not involve technologically demanding equipment. Most SABRE polarization studies have been done using methanol-d4 as a solvent, which is not suitable for in vivo application. The main goal of this work was to obtain hyperpolarized pyruvate in a solvent other than methanol which may open the door to further purification steps and enable a method to polarize pyruvate in water in future. This work demonstrates hyperpolarization of the [2-13C]pyruvate as well as [1-13C]pyruvate by SABRE in an acetone/water solvent system at room temperature as an alternative to methanol, which is commonly used. NMR signals are detected using a 1.1 T benchtop NMR spectrometer. In this work we have primarily focused on the study of [2-13C]pyruvate and investigated the effect of catalyst concentration, DMSO presence and water vs. acetone solvent concentration on the signal enhancement. The relaxation times for [2-13C]-pyruvate solutions are reported in the hope of informing the development of future purification methods. [ABSTRACT FROM AUTHOR]

Response surface methodology (RSM) was used to optimize the extraction process of naringin. The central component design included three parameters of extraction, namely temperature (X1), solid–liquid ratio (X2), and extraction time (X3). The optimum extraction temperature was 67 °C; the ratio of feed to solvent was 54:1 mL/g, and the extraction time was 2.8 h. According to the best extraction conditions, naringin was processed to verify the accuracy of the model. Five parallel experiments were set up, and a yield of 3.248% naringin was obtained, which was equivalent to the predicted yield of 3.256%. Naringin was purified to obtain naringin-refined products using DM101 macroporous adsorption resin. Naringin dihydrochalcone was synthesized following catalytic hydrogenation of purified naringin. The structures of naringin and naringin dihydrochalcone were determined via Fourier infrared spectrometer and nuclear magnetic resonance spectrometry. In vitro determination of the lipid-lowering activity of naringin dihydrochalcone was also conducted. Further focusing on HepG2 cells, a high cholesterol-induced high-fat HepG2 cell model was established. We measured the effects of different concentrations of naringin dihydrochalcone on intracellular lipids in denatured HepG2 cells and further validated the lipid-lowering effect of naringin at the cellular level. The results showed that naringin dihydrochalcone has a potential application in functional foods for lowering blood lipids. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance relaxation of the proton spins of liquid molecules and their evolution during processes such as drying, fluid flow, and phase change of a sample can be monitored in a nondestructive way. A unilateral 1H NMR sensor made with a permanent magnet array, inspired by the NMR MOUSE, with an RF coil tuned to 11.71 MHz was developed. This creates a sensitive homogeneous measuring volume parallel to the sensor surface and located 14 mm from its surface, allowing contactless measurements from the sample's interior. As this sensitive volume is moved across the sample using a semi-automatic linear displacement mechanism with millimetric precision, spatial T2 lifetime and signal intensity 1D profiles can be obtained. To characterize the sensor's sensitive volume, eraser samples were used. To evaluate the sensor's ability to characterize different materials, cement paste samples containing ordinary and white Portland cement were prepared and measured at seven days of age. In addition, measurements were made on organic samples such as a Hass avocado and beef steak. Based on the results, a 1 mm spatial resolution of the sensor was achieved. The sensor was able to detect differences in T2 lifetimes in eraser specimens composed of layers of three different erasers. Also, a clear difference in T2 lifetimes and signal intensities was observed in cement pastes composed of white and ordinary Portland cement. On the other hand, it was possible to obtain signals from the peel and pulp of the avocado fruit, as well as from the fat and meat in a beef steak in a nondestructive way. The T2 lifetimes of the different materials agreed with those obtained using a commercial NMR spectrometer. [ABSTRACT FROM AUTHOR]

The dechlorination of epoxidized Cardol (E‐Cardol), which is a high‐performance and sustainable adhesive and packaging material for electronics, remains challenging. The previous work proposed a new alcohol‐sodium refining method to efficiently remove the chlorine of E‐Cardol. However, this method is strongly limited by the trade‐off between the dechlorination efficiency and its polymerization side effect, which leads to the viscosity as well as the epoxy equivalent increase of E‐Cardol. Based on the detailed analysis of the refining process using fourier transform infrared spectroscopy (FTIR), simultaneous thermal analysis (STA), and nuclear magnetic resonance spectrometer (NMR) epoxidized Cardol (E‐Cardol), this trade‐off is studied. It is found that the dechlorination efficiency increases with the increase of the usage of the alcohol sodium. Meanwhile, when the residual alcohol‐sodium content after refining exceeds 3000 ppm, the viscosity of the E‐Cardol increases significantly due to the increased polymerization of E‐Cardol by epoxy ring‐opening reaction. It is demonstrated that the alcohol‐sodium refining method can efficiently reduce the chlorine content of E‐Cardol with the initial hydrolyzable chlorine content not higher than 3000 ppm to below 300 ppm without influencing their epoxy equivalent and viscosity. This paper thoroughly explores the mechanism and application range of the proposed alcohol‐sodium refining method, which is crucial for the facile preparation of electronic‐grade E‐Cardol materials. [ABSTRACT FROM AUTHOR]

The present study investigated the 1H Nuclear Magnetic Resonance (NMR) spectra of hydrogen-rich water (HRW) produced using the EVObooster device. The analyzed HRW has pH = 7.1 ± 0.11, oxidation–reduction potential (ORP) of (−450 ± 11) mV, and a dissolved hydrogen concentration of 1.2 ppm. The control sample was tap water filtered by patented technology. A 600 NMR spectrometer was used to measure NMR spectra. Isotropic 1H nuclear magnetic shielding constants of the most stable clusters (H2O)n with n from 3 to 28 have been calculated by employing the gauge-including-atomic-orbital (GIAO) method at the MPW1PW91/6-311+G(2d,p) density function level of theory (DFT). The HRW chemical shift is downfield (higher chemical shifts) due to increased hydrogen bonding. More extensive formations were formed in HRW than in control filtered tap water. The exchange of protons between water molecules is rapid in HRW, and the 1H NMR spectra are in fast exchange mode. Therefore, we averaged the calculated chemical shifts of the investigated water clusters. As the size of the clusters increases, the number of hydrogen bonds increases, which leads to an increase in the chemical shift. The dependence is an exponential saturation that occurs at about N = 10. The modeled clusters in HRW are structurally stabilized, suggesting well-ordered hydrogen bonds. In the article, different processes are described for the transport of water molecules and clusters. These processes are with aquaporins, fusion pores, gap-junction channels, and WAT FOUR model. The exponential trend of saturation shows the dynamics of water molecules in clusters. In our research, the chemical shift of 4.257 ppm indicates stable water clusters of 4–5 water molecules. The pentagonal rings in dodecahedron cage H3O+(H2O)20 allow for an optimal arrangement of hydrogen bonds that minimizes the potential energy. [ABSTRACT FROM AUTHOR]

ABSTRACT HRMAS (high‐resolution magic angle spinning) nuclear magnetic resonance (NMR) spectroscopy of low‐density polyethylene (LDPE) affords 1H and 13C NMR spectra with superior resolution. For acquiring HRMAS NMR spectra, the polymer is first swollen with representative organic solvents. Then, the samples are measured with a conventional solid‐state NMR spectrometer in the wideline mode or at the low spinning speed of 2 kHz. Anisotropic interactions like CSA (chemical shift anisotropy) and dipolar interactions are reduced due to the additional mobility of the polymer chains in the presence of the solvent within the polymer network. The combined effect of this mobility and MAS leads to signals with substantially reduced halfwidths as compared to classic MAS of the dry polymer. With HRMAS, all signals of the polymer become visible, and the spectra can be used for a quick and easy assessment of the polymer swelling behavior in diverse solvents. Being able to characterize polymers on the molecular level, and identifying the solvents that penetrate the polymer network best, enables the study of post‐synthesis modifications of the polymers. It is demonstrated by paramagnetic HRMAS that the metallocene nickelocene (Cp2Ni) penetrates the LDPE network along with the solvent and is homogeneously dispersed in the polymer. SEM images prove that the structure of the polymer is not altered by the presence of a solvent and Cp2Ni. The impact of the paramagnetic Cp2Ni on the 1H signal halfwidth and T1 time of LDPE is studied. HRMAS allows a quick assessment of metal complexes regarding their ability to penetrate the LDPE network and therefore supports future studies of catalytic polymer degradation. [ABSTRACT FROM AUTHOR]

This article presents the preparation of environmentally friendly water‐soluble lubricant additives. Adipic acid (AA), sebacic acid (SA) and dodecanedioic acid (DA) were individually subjected to esterification reactions with polyethylene glycol 1500 (PEG1500) to prepare a class of water‐soluble polyether esters (AAPEE1500, SAPEE1500 and DAPEE1500) (referred to as XAPEE1500s) that exhibit excellent water solubility and do not contain environmentally harmful elements. First, the molecular structure characterisation and functional group analysis of these additives will be conducted using an infrared spectrometer and a nuclear magnetic resonance spectrometer. Subsequently, the frictional properties of the additives in the base liquid (deionised water) will be investigated using an SRV‐V tribometer, Falex pin‐on‐disc tribometer and screw torque tester. The surface morphology of wear scars will be characterised and analysed using scanning electron microscopy (SEM) and a non‐contact 3D profilometer. Finally, the lubrication mechanism of the DAPEE1500 additive will be analysed using X‐ray photoelectron spectroscopy (XPS). The results indicate that the optimal lubrication performance is achieved when the added mass fraction of DAPEE1500 is at 3%. Compared with 0.5 wt% DAPEE1500, the average friction coefficient of 3 wt% DAPEE1500 decreased from 0.285 to 0.122, and the wear volume decreased from 25.52 × 10−5 μm3 to 10.96 × 10−5 μm3. The lubrication mechanism of polyether ester is the result of the combined action of its polar ester functional groups and long carboxylic acid chains in the structure. These polar functional groups can form a relatively firm adsorption film on the friction surface, while the long carboxylic acid chains act as a brush‐like isolating layer, thus demonstrating superior anti‐wear and anti‐friction performance. [ABSTRACT FROM AUTHOR]

The spatial resolution in magnetic resonance imaging is mainly limited by low SNR, which is commonly addressed by long measurement times or dedicated hardware. In single digit micron resolutions, diffusion becomes a further limiting factor since depending on the gradient strength, the diffusion length of particles may approach the target resolutions. Spatial resolution improvement has been addressed by microscopy inserts comprising dedicated gradient systems and RF-coils, usually designed for NMR spectrometers that are often equipped with a deuterium lock for field drift compensations. The presented microscopy insert has been designed to provide single-digit micron resolutions on horizontal preclinical imaging systems utilizing their full imaging and user interface capabilities. The incorporated gradient provides an efficiency of 0.135 T/(m∙A) which in combination with the system's gradient amplifiers yields a maximum of 27 T/m. With the additional low noise amplifier added to the RF-path a three-fold SNR improvement could be achieved for small samples. Furthermore, a modified constant time imaging sequence was introduced to improve the capability of the setup for ultra‐high-resolution imaging demonstrated on zebrafish embryos at different development stages with (9 μm)³ resolution. [ABSTRACT FROM AUTHOR]

The possibility of changing the efficiency of nuclear spin–phonon coupling by NMR methods using the example of a NaF crystal in a wide temperature range is investigated. To suppress nuclear spin-lattice relaxation involving paramagnetic centers, continuous magnetic saturation at a single Larmor frequency is used instead of acoustic saturation of the 23Na NMR signal at a double frequency. The influence of the (i) color centers induced by gamma irradiation and (ii) temperature on the separation of spin–phonon coupling mechanisms is studied. No suppression of impurity relaxation is observed for 19F dipole nuclei. It is shown that the suggested magnetic saturation technique for complete or partial shutdown of impurity relaxation of quadrupole nuclei can be implemented on commercial pulse NMR spectrometers. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance (NMR) is recognized as the gold standard method in fragment‐based drug design for screening, hit validation, and affinity determination. However, its deployment at a large scale is limited by the cost and expertise needed to implement NMR as a routine drug discovery method. The increase in the adoption of fragment‐based drug design created a need for biophysics to provide high‐quality data for weak ligand‐target interactions that can be implemented at scale. NMR must adapt its position in drug design operations to enter this new era. The recent development of commercially available benchtop NMR spectrometers in combination with hyperpolarization methods represents an opportunity for highly deployable and scalable systems. [ABSTRACT FROM AUTHOR]

Hypoxic‐ischemic encephalopathy (HIE) is a common neurological syndrome in newborns with high mortality and morbidity. Therapeutic hypothermia (TH), which is standard of care for HIE, mitigates brain injury by suppressing anaerobic metabolism. However, more than 40% of HIE neonates have a poor outcome, even after TH. This study aims to provide metabolic biomarkers for predicting the outcomes of hypoxia‐ischemia (HI) after TH using hyperpolarized [1‐13C] pyruvate magnetic resonance spectroscopy. Postnatal day 10 (P10) mice with HI underwent TH at 1 h and were scanned at 6–8 h (P10), 24 h (P11), 7 days (P17), and 21 days (P31) post‐HI on a 14.1‐T NMR spectrometer. The metabolic images were collected, and the conversion rate from pyruvate to lactate and the ratio of lactate to pyruvate in the injured left hemisphere (kPL(L) and Lac/Pyr(L), respectively) were calculated at each timepoint. The outcomes of TH were determined by the assessments of brain injury on T2‐weighted images and behavioral tests at later timepoint. kPL(L) and Lac/Pyr(L) over time between the good‐outcome and poor‐outcome groups and across timepoints within groups were analyzed. We found significant differences in temporal trends of kPL(L) and Lac/Pyr(L) between groups. In the good‐outcome group, kPL(L) increased until P31 with a significantly higher value at P31 compared with that at P10, while the level of Lac/Pyr(L) at P31 was notably higher than those at all other timepoints. In the poor‐outcome group, kPL(L) and Lac/Pyr(L) increased within 24 h. The kPL(L) value at P11 was considerably higher compared with P10. Discrete temporal changes of kPL(L) and Lac/Pyr(L) after TH between the good‐outcome and poor‐outcome groups were seen as early as 24 h after HI, reflecting various TH effects on brain anaerobic metabolism, which may provide insights for early screening for response to TH. [ABSTRACT FROM AUTHOR]

SABRE is emerging as a fast, simple and low-cost hyperpolarization method because of its ability to regenerate enhanced NMR signals. Generally, SABRE hyperpolarization has been performed predominantly manually, leading to variations in reproducibility and efficiency. Recent advances in SABRE include the development of automated shuttling systems to address previous inconsistencies. However, the operational complexity of such systems and the challenges of integration with existing workflows hinder their widespread adoption. This work presents a fully automated lab workstation based on a benchtop NMR spectrometer, specifically designed to facilitate SABRE of different nuclei across different polarization fields. We demonstrated the capability of this system through a series of routine SABRE experimental protocols, including consecutive SABRE hyperpolarization with high reproducibility (average standard deviation of 1.03%), optimization polarization of 13C nuclei respect to the polarization transfer field, and measurement of polarization buildup rate or decay time across a wide range of magnetic fields. Furthermore, we have iteratively optimized the durations for pulsed SABRE-SHEATH 13C pyruvate. The constructed SABRE workstation offers full automation, high reproducibility, and functional diversification, making it a practical tool for conducting routine SABRE hyperpolarization experiments. It provides a robust platform for high-throughput and reliable SABRE and X-SABRE hyperpolarization studies. [ABSTRACT FROM AUTHOR]

This article, published in the Chemistry of Natural Compounds journal, explores the secondary metabolites of Cinnamomum burmanni, a spice commonly used in Indonesia. The study identifies 22 compounds from the stems of the plant, including triterpenoids, coumarins, steroids, benzenoids, lignans, oxysporones, and apocarotenoids. Many of these compounds are reported for the first time in this plant. The article provides detailed information on the extraction and isolation methods used, as well as the physical and spectroscopic properties of the compounds. The document also acknowledges the support of Yuan's General Hospital for the investigation. Overall, this report offers valuable insights into the chemical composition of Cinnamomum burmanni and is a useful resource for library patrons conducting research in this area. [Extracted from the article]

Today, it is difficult to have a high-field nuclear magnetic resonance (NMR) device due to the high cost of its acquisition and maintenance. These high-end machines require significant space and specialist personnel for operation and offer exceptional quality in the acquisition, processing, and other advanced functions associated with detected signals. However, alternative devices are low-field nuclear magnetic resonance devices. They benefit from the elimination of high-tech components that generate static magnetic fields and advanced instruments. Instead, they used magnetic fields induced by ordinary conductors. Another category of spectrometers uses the Earth's magnetic field, which is simple and economical but limited in use. These devices are called Earth-Field Nuclear Magnetic Resonance (EFNMR) devices. This device is ideal for educational purposes, especially for engineers and those who study nuclear magnetic resonance, such as chemistry or other experimental sciences. Students can observe their internal workings and conduct experiments that complement their education without worrying about damaging equipment. This article provides a detailed explanation of the design and construction of electrical technology devices for the excitation of atomic spin resonance using Earth's magnetic fields. It covers all necessary stages, from research to analysis, including simulation, assembly, construction of each component, and the development of comprehensive software for spectrometer control. [ABSTRACT FROM AUTHOR]

Deuterium (2H) spin relaxation of 13CH2D methyl groups has been widely applied to investigate picosecond-to-nanosecond conformational dynamics in proteins by solution-state NMR spectroscopy. The B0 dependence of the 2H spin relaxation rates is represented by a linear relationship between the spectral density function at three discrete frequencies J(0), J(ωD) and J(2ωD). In this study, the linear relation between 2H relaxation rates at B0 fields separated by a factor of two and the interpolation of rates at intermediate frequencies are combined for a more robust approach for spectral density mapping. The general usefulness of the approach is demonstrated on a fractionally deuterated (55%) and alternate 13C-12C labeled sample of E. coli RNase H. Deuterium relaxation rate constants (R1, R1ρ, RQ, RAP) were measured for 57 well-resolved 13CH2D moieties in RNase H at 1H frequencies of 475 MHz, 500 MHz, 900 MHz, and 950 MHz. The spectral density mapping of the 475/950 MHz data combination was performed independently and jointly to validate the expected relationship between data recorded at B0 fields separated by a factor of two. The final analysis was performed by jointly analyzing 475/950 MHz rates with 700 MHz rates interpolated from 500/900 MHz data to yield six J(ωD) values for each methyl peak. The J(ω) profile for each peak was fit to the original (τM, Sf2, τf) or extended model-free function (τM, Sf2, Ss2, τf, τs) to obtain optimized dynamic parameters. [ABSTRACT FROM AUTHOR]

Neurofibrillary tangles of tau constitute one of the key biological hallmarks of Alzheimer's disease. Currently, the assessment of regional tau accumulation requires intravenous administration of radioactive tracers for PET imaging. A noninvasive MRI‐based solution would have significant clinical implications. Herein, we utilized an MRI technique known as chemical exchange saturation transfer (CEST) to determine the imaging signature of tau in both its monomeric and pathologic fibrillated conformations. Three sets of purified recombinant full‐length (4R) tau protein were prepared for collection of CEST spectra using a 9.4 T NMR spectrometer at varying temperatures (25, 37, and 42 °C) and RF intensities (0.7, 1.0, 1.5, and 2.2 μT). Monomeric and fibrillated tau were readily distinguished based on their Z‐spectrum profiles. Fibrillated tau demonstrated a less prominent peak at 3.5 ppm with additional peaks near 0.5 and 1.5 ppm. No significant differences were identified between fibrillated tau prepared using heparin versus seed‐competent tau. In conclusion, monomeric and fibrillated tau can be readily detected and distinguished based on their CEST‐derived Z‐spectra, pointing to the potential utility of CEST‐MRI as a noninvasive biomarker of regional pathologic tau accumulation in the brain. Further testing and validation in vitro and in vivo will be necessary before this can be applied clinically. [ABSTRACT FROM AUTHOR]

Poly (vinyl chloride) (PVC) films modified with ethylenediamine (en) and doped by nanoparticles (TiO2, ZnO, NiO, and MgO). A mixture of 0.5 g PVC/en dissolved in THF and 0.01 wt % of nanoparticles were used in doping PVC to produce the nanocomposite films. All modified PVC films were characterized by different analysis techniques such as Fourier Transform Infrared (FTIR), Nuclear Magnetic Resonance Spectrometer (NMR), diffusive reflectance spectroscopy (DRS), X‐ray diffraction analysis (XRD), and scanning electron microscopy (SEM). The DRS was used to analyse the scattered IR energy of the samples at wavelengths between (250–1350 nm). The optical properties and oscillator strength were also studied, the transmittance and reflectance values declined for the PVC films, and the absorption coefficient was observed between (79–89 %). The direct energy gap decreased from 4.6 to 1.9, and the indirect energy gap reduced from 4.3 to 1.9. The XRD exhibited a semi‐crystalline structure and the SEM test exhibited a porous structure of all samples. The Urbach energy was increased from 0.8772 eV to 14.712 eV, single oscillator energy (Eo ${{E}_{o}}$) was also increased from 6.38 eV to 13.69 eV and the dispersion energy (Ed) ${{(E}_{d})}$ increased from 23.40 eV to 70.63 eV. Moreover, the surface roughness parameters Ra and Rq of the PVC films in modified and doping were increased from 3.86 nm to 8.14 nm, and 5.08 nm to 10.10 nm respectively. So, PVC results show increased optical properties after modification with en and doping by NPs are used in the light conversion and aerospace industries. [ABSTRACT FROM AUTHOR]

Multilayered plastics are widely used in food packaging and other commercial applications due to their tailored functional properties. By layering different polymers, the multilayered composite material can have enhanced mechanical, thermal, and barrier properties compared to a single plastic. However, there is a significant need to recycle these multilayer plastics, but their complex structure offers significant challenges to their successful recycling. Ultimately, the use and recycling of these complex materials requires the ability to characterize the composition and purity as a means of quality control for both production and recycling processes. New advances and availability of low‐field benchtop 1H NMR spectrometers have led to increasing interest in its use for characterization of multicomponent polymers and polymer mixtures. Here, we demonstrate the capability of low‐field benchtop 1H NMR spectroscopy for characterization of three common polymers associated with multilayered packaging systems (low‐density polyethylene [LDPE], ethylene vinyl alcohol [EVOH], and Nylon) as well as their blends. Calibration curves are obtained for determining the unknown composition of EVOH and Nylon in multilayered packaging plastics using both the EVOH hydroxyl peak area and an observed peak shift, both yielding results in good agreement with the prepared sample compositions. Additionally, comparison of results extracted for the same samples characterized by our benchtop spectrometer and a 500‐MHz spectrometer found results to be consistent and within 2 wt% on average. Overall, low‐field benchtop 1H NMR spectroscopy is a reliable and accessible tool for characterization of these polymer systems. [ABSTRACT FROM AUTHOR]

Epimedium brevicornu Maxim (E. brevicornu) is a plant of Epimedium L. in Berberidaceae, which is widely distributed and has high medicinal value and many important clinical applications. In this experiment, a novel flavonoid compound (1) was isolated and identified the chemical structure from E. brevicornu. The extract of E. brevicornu was performed on normal silica column chromatography, ODS silica column chromatography, Sephadex LH-20 column chromatography and RP-HPLC system to be isolated and purified and obtained 1. The HR-ESI-MS and NMR spectrometer were used to measure the accuracy molecular weights and determine the chemical structure of 1. In conclusion, we isolated and purified compound 1 (15.4 mg) and determined its chemical structure. [ABSTRACT FROM AUTHOR]

Benchtop nuclear magnetic resonance (NMR) spectrometers are being employed in a wide variety of applications from undergraduate teaching and research in academia to quality control and process monitoring in industrial settings. Incorporating benchtop NMR in some of these applications presents opportunities for new practical uses of the technology and challenges that truly test the capabilities of compact NMR spectrometers. For instance, the use of protonated solvents in manufacturing or process monitoring requires separating and quantitating the analyte signals of interest from the strong (overwhelming) response from the solvents. Furthermore, due to the lower field strength available with permanent magnet spectrometers, the NMR spectra of complex mixtures can be more difficult to analyze due to partial or complete signal overlap. To address some of these challenges and to extend the range of applications of benchtop NMR, we investigate NMR techniques that enable quantitative analysis of different components in mixtures. These pulse sequences can be used to suppress one or multiple solvent peaks, to filter out signals by spin–spin relaxation time (T2), or to separate signal components by a molecule's diffusion coefficient (NMR diffusometry). In this paper, we discuss quantitative analysis of excipients in buffers for therapeutic proteins to highlight the usefulness of these NMR pulse sequences in the analysis of complex samples with benchtop NMR spectrometers. [ABSTRACT FROM AUTHOR]

The discovery of new ceramic materials containing Ba‐La‐Cu oxides in 1986 that exhibited superconducting properties at high temperatures in the range of 35 K or higher, recognized with the Nobel Prize in Physics in 1987, opened a new world of opportunities for nuclear magnetic resonance (NMRs) and magnetic resonance imaging (MRIs) to move away from liquid cryogens. This discovery expands the application of high temperature superconducting (HTS) materials to fields beyond the chemical and medical industries, including electrical power grids, energy, and aerospace. The prototype 400‐MHz cryofree HTS NMR spectrometer installed at Amgen's chemistry laboratory has been vital for a variety of applications such as structure analysis, reaction monitoring, and CASE‐3D studies with RDCs. The spectrometer has been integrated with Amgen's chemistry and analytical workflows, providing pipeline project support in tandem with other Kinetic Analysis Platform technologies. The 400‐MHz cryofree HTS NMR spectrometer, as the name implies, does not require liquid cryogens refills and has smaller footprint that facilitates installation into a chemistry laboratory fume hood, sharing the hood with a process chemistry reactor. Our evaluation of its performance for structural analysis with CASE‐3D protocol and for reaction monitoring of Amgen's pipeline chemistry was successful. We envision that the HTS magnets would become part of the standard NMR and MRI spectrometers in the future. We believe that while the technology is being developed, there is room for all magnet options, including HTS, low temperature superconducting (LTS) magnets, and low field benchtop NMRs with permanent magnets, where utilization will be dependent on application type and costs. [ABSTRACT FROM AUTHOR]

Pancakes prepared with sorghum flour possess a high nutritional value, yet their quality is unstable and prone to degradation during storage. This instability can be attributed to the particle size of coarse cereal powder, which significantly influences the quality of flour products during storage. In this study, changes in the quality of these pancakes, prepared with varying particle sizes of sorghum flour, were meticulously analyzed during cold storage using advanced instruments such as a texture analyzer, nuclear magnetic resonance spectrometer, differential scanning calorimeter, X-ray diffractometer, and Fourier transform infrared spectrometer. Findings revealed that the hardness of leavened pancakes significantly increased over time. After a refrigeration period of 7 days, the hardness of wheat flour leavened pancakes increased by 56.60%. However, with a decrease in the particle size of sorghum flour, the increase in hardness diminished, thereby delaying the aging process of the pancakes. As the storage duration was extended, moisture migration within the pancakes occurred, and the sorghum flour pancakes with a smaller particle size exhibited a reduced moisture change rate, indicating an enhanced water holding capacity. In comparison to their wheat flour counterparts, sorghum flour leavened pancakes exhibited a substantial reduction in retrogradation enthalpy and crystallinity. The inclusion of sorghum flour effectively inhibited amylopectin recrystallization, thus slowing down the aging process of the pancakes. This inhibitory effect was more evident with decreasing sorghum flour particle sizes. Fourier transform infrared data indicated no significant alterations in absorption peaks across various wavelengths during cold storage. Although starch short-range orderliness increased with storage time, the use of sorghum flour with smaller particles reduced the degree of short–range orderliness in starch molecules throughout the cold storage period. Sorghum flour with a smaller particle size can inhibit water migration and amylopectin recrystallization, which subsequently delays pancake aging and enhances its quality stability during storage. [ABSTRACT FROM AUTHOR]

Controlling the enantiomeric purity of chiral drugs is of paramount importance in pharmaceutical chemistry. Isotropic 1H NMR spectroscopy involving chiral agents is a widely used method for discriminating enantiomers and quantifying their relative proportions. However, the relatively weak spectral separation of enantiomers (1H Δδiso(R, S)) in frequency units at low and moderate magnetic fields, as well as the lack of versatility of a majority of those agents with respect to different chemical functions, may limit the general use of this approach. In this article, we investigate the analytical potential of 19F NMR in anisotropic chiral media for the enantiomeric analysis of fluorinated active pharmaceutical ingredients (API) via two residual anisotropic NMR interactions: the chemical shift anisotropy (19F-RCSA) and dipolar coupling ((19F-19F)- RDC). Lyotropic chiral liquid crystals (CLC) based on poly-γ-benzyl-L-glutamate (PBLG) show an interesting versatility and adaptability to enantiodiscrimination as illustrated for two chiral drugs, Flurbiprofen® (FLU) and Efavirenz® (EFA), which have very different chemical functions. The approach has been tested on a routine 300 MHz NMR spectrometer equipped with a standard probe (5 mm BBFO probe) in a highthroughput context (i.e., ≈10 s of NMR experiments) while the performance for enantiomeric excess (ee) measurement is evaluated in terms of trueness and precision. The limits of detection (LOD) determined were 0.17 and 0.16 µmol ml-1 for FLU and EFA, respectively, allow working in dilute conditions even with such a short experimental duration. The enantiodiscrimination capabilities are also discussed with respect to experimental features such as CLC composition and temperature. [ABSTRACT FROM AUTHOR]

In‐situ NMR spectroscopy can provide valuable insight into chemical reactions, including detailed information on reaction kinetics and thus mechanism. The application of in‐situ NMR techniques to heterogeneous reactions has so far been limited by the requirement for efficient mixing, which is challenging within the confines of a standard NMR spectrometer. We report an automated plunger‐based device for the mixing of heterogeneous solid‐liquid reactions conducted within a 5 mm tube in a standard NMR probe, allowing reaction kinetics and speciation to be monitored in‐situ. The system has been tested by measuring the kinetics for three diverse reactions and comparison of these with the reaction velocities measured by routine ex‐situ analysis after sampling. The effect of key parameters including plunger design, plunger velocity, solid settling time, and mixing‐to‐acquisition time ratio are explored to determine the optimum parameters for combining efficient mixing with spectral quality. With adaptation, the device may also be suitable for benchtop NMR. [ABSTRACT FROM AUTHOR]

Benchtop NMR spectroscopy is attractive for process monitoring; however, there are still drawbacks that often hamper its use, namely, the comparatively low spectral resolution in 1H NMR, as well as the low signal intensities and problems with the premagnetization of flowing samples in 13C NMR. We show here that all these problems can be overcome by using 1H‐13C polarization transfer methods. Two ternary test mixtures (one with overlapping peaks in the 1H NMR spectrum and one with well‐separated peaks, which was used as a reference) were studied with a 1 T benchtop NMR spectrometer using the polarization transfer sequence PENDANT (polarization enhancement that is nurtured during attached nucleus testing). The mixtures were analyzed quantitatively in stationary as well as in flow experiments by PENDANT enhanced 13C NMR experiments, and the results were compared with those from the gravimetric sample preparation and from standard 1H and 13C NMR spectroscopy. Furthermore, as a proxy for a process monitoring application, continuous dilution experiments were carried out, and the composition of the mixture was monitored in a flow setup by 13C NMR benchtop spectroscopy with PENDANT. The results demonstrate the high potential of polarization transfer methods for applications in quantitative process analysis with benchtop NMR instruments, in particular with flowing samples. [ABSTRACT FROM AUTHOR]

Efficient and robust analytical methods are needed to improve the identification and subsequent regulation of new psychoactive substances (NPS). NMR spectroscopy is a unique method able to determine the structure of small molecules such as NPS even in mixtures. However, high‐field NMR analysis is associated with expensive purchase and maintenance costs. For more than a decade, compact NMR spectrometers have changed this paradigm. It was recently shown that a dedicated analytical workflow combining compact NMR and databases could identify the molecular structure of NPS, in spite of the lower spectral dispersion and sensitivity of compact spectrometers. This approach relies on 1H‐13C HSQC to both recognize NPS and elucidate the structure of unknown substances. Still, its performance is limited by the need to compromise between resolution and experiment time. Here, we show that this strategy can be significantly improved by implementing non‐uniform sampling (NUS) to improve spectral resolution in the 13C dimension of HSQC at no cost in terms of experiment time. Gains in the range of 3 to 4 in resolution are achieved for pure NPS and for a mixture. Finally, 2D HSQC with NUS was applied to improve the identification of NPS with the assistance of databases. The resulting method appears as a useful tool for the characterization of NPS in mixtures, which is essential for forensic laboratories. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance (NMR) is an established method to determine self‐diffusion coefficients in liquids with high precision. The development of benchtop NMR spectrometers makes the method accessible to a wider community. In most cases, 1H NMR spectroscopy is used to determine self‐diffusion coefficients due to its high sensitivity. However, especially when using benchtop NMR spectrometers for the investigation of complex mixtures, the signals in 1H NMR spectra can overlap, hindering the precise determination of self‐diffusion coefficients. In 13C NMR spectroscopy, the signals of different compounds are generally well resolved. However, the sensitivity of 13C NMR is significantly lower than that of 1H NMR spectroscopy leading to very long measurement times, which makes diffusion coefficient measurements based on 13C NMR practically infeasible with benchtop NMR spectrometers. To circumvent this problem, we have combined two known pulse sequences, one for polarization transfer from 1H to the 13C nuclei (PENDANT) and one for the measurement of diffusion coefficients (PFG). The new method (PENPFG) was used to measure the self‐diffusion coefficients of three pure solvents (acetonitrile, ethanol and 1‐propanol) as well as in all their binary mixtures and the ternary mixture at various compositions. For comparison, also measurements of the same systems were carried out with a standard PFG‐NMR routine on a high‐field NMR instrument. The results are in good agreement and show that PENPFG is a useful tool for the measurement of the absolute value of the self‐diffusion coefficients in complex liquid mixtures with benchtop NMR spectrometers. [ABSTRACT FROM AUTHOR]

Recently, benchtop nuclear magnetic resonance (NMR) spectrometers utilizing permanent magnets have emerged as versatile tools with applications across various fields, including food and pharmaceuticals. Their efficacy is further enhanced when coupled with chemometric methods. This study presents an innovative approach to leveraging a compact benchtop NMR spectrometer coupled with chemometrics for screening honey-based food supplements adulterated with active pharmaceutical ingredients. Initially, fifty samples seized by French customs were analyzed using a 60 MHz benchtop spectrometer. The investigation unveiled the presence of tadalafil in 37 samples, sildenafil in 5 samples, and a combination of flibanserin with tadalafil in 1 sample. After conducting comprehensive qualitative and quantitative characterization of the samples, we propose a chemometric workflow to provide an efficient screening of honey samples using the NMR dataset. This pipeline, utilizing partial least squares discriminant analysis (PLS-DA) models, enables the classification of samples as either adulterated or non-adulterated, as well as the identification of the presence of tadalafil or sildenafil. Additionally, PLS regression models are employed to predict the quantitative content of these adulterants. Through blind analysis, this workflow allows for the detection and quantification of adulterants in these honey supplements. [ABSTRACT FROM AUTHOR]

NMR spectroscopy is one of the most potent methods in analytical chemistry. NMR titration experiments are particularly useful since they measure molecular binding affinities and other concentration-dependent effects. These experiments, however, require a long series of measurements. An alternative to these serial measurements has recently been presented, exploiting a pH (or generally – a concentration) gradient along the NMR tube. The proposed experiment, although efficient, was based on the sensitivity- and hardware-demanding chemical shift imaging (CSI) method. Thus, it is practically limited to high-resolution NMR spectrometers. This paper proposes modifying and adapting the approach to the popular and cost-efficient benchtop NMR machines. Instead of CSI, we use a device that shifts the NMR tube vertically to measure the spectra of different sample volumes, which have different pH values due to the established gradient along the tube. We demonstrate the potential of the method on the test samples of L -tyrosine and 2,6-lutidine, and two real samples from the food industry – an infant formula and an energy drink. The proposed method boosts spectral resolution and allows for the sampling of a broader range of pH values when compared to the original approach. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance (NMR) spectroscopy is a powerful tool for qualitative and quantitative analysis. However, for complex mixtures, determining the speciation from NMR spectra can be tedious and sometimes even unfeasible. On the other hand, identifying and quantifying structural groups in a mixture from NMR spectra is much easier than doing the same for components. We call this group‐based approach "NMR fingerprinting." In this work, we show that NMR fingerprinting can even be performed in an automated way, without expert knowledge, based only on standard NMR spectra, namely, 13C, 1H, and 13C DEPT NMR spectra. Our approach is based on the machine‐learning method of support vector classification (SVC), which was trained here on thousands of labeled pure‐component NMR spectra from open‐source data banks. We demonstrate the applicability of the automated NMR fingerprinting using test mixtures, of which spectra were taken using a simple benchtop NMR spectrometer. The results from the NMR fingerprinting agree remarkably well with the ground truth, which was known from the gravimetric preparation of the samples. To facilitate the application of the method, we provide an interactive website (https://nmr-fingerprinting.de), where spectral information can be uploaded and which returns the NMR fingerprint. The NMR fingerprinting can be used in many ways, for example, for process monitoring or thermodynamic modeling using group‐contribution methods—or simply as a first step in species analysis. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance (NMR) spectroscopy is a powerful analytical technique with the ability to acquire both quantitative and structurally insightful data for multiple components in a test sample. This makes NMR spectroscopy a desirable tool to understand, monitor, and optimize chemical transformations. While quantitative NMR (qNMR) approaches relying on internal standards are well‐established, using an absolute external calibration scheme is beneficial for reaction monitoring as resonance overlap complications from an added reference material to the sample can be avoided. Particularly, this type of qNMR technique is of interest with benchtop NMR spectrometers as the likelihood of resonance overlap is only enhanced with the lower magnetic field strengths of the used permanent magnets. The included study describes a simple yet robust methodology to determine concentration conversion factors for NMR systems using single‐ and multi‐analyte linear regression models. This approach is leveraged to investigate a pharmaceutically relevant amide coupling batch reaction. An on‐line stopped‐flow (i.e., interrupted‐flow or paused‐flow) benchtop NMR system was used to monitor both the 1,1′‐carbonyldiimidazole (CDI) promoted acid activation and the amide coupling. The results highlight how quantitative measurements in benchtop NMR systems can provide valuable information and enable analysts to make decisions in real time. [ABSTRACT FROM AUTHOR]

The neuropathological sequelae of stroke and subsequent recovery are incompletely understood. Here, we investigated the metabolic dynamics following stroke to advance the understanding of the pathophysiological mechanisms orchestrating stroke recovery. Using a nuclear magnetic resonance (NMR)-driven metabolomic profiling approach for urine samples obtained from a clinical group, the objective of this research was to (1) identify novel biomarkers indicative of severity and recovery following stroke, and (2) uncover the biochemical pathways underlying repair and functional recovery after stroke. Urine samples and clinical stroke assessments were collected during the acute (2–11 days) and chronic phases (6 months) of stroke. Using a 700 MHz 1H NMR spectrometer, metabolomic profiles were acquired followed by a combination of univariate and multivariate statistical analyses, along with biological pathway analysis and clinical correlations. The results revealed changes in phenylalanine, tyrosine, tryptophan, purine, and glycerophospholipid biosynthesis and metabolism during stroke recovery. Pseudouridine was associated with a change in post-stroke motor recovery. Thus, NMR-based metabolomics is able to provide novel insights into post-stroke cellular functions and establish a foundational framework for future investigations to develop targeted therapeutic interventions, advance stroke diagnosis and management, and enhance overall quality of life for individuals with stroke. [ABSTRACT FROM AUTHOR]

The design of biocompatible cell culture substrates and electrospun nanofibers can improve cell proliferation and behavior in laboratory conditions for tissue engineering applications in medicine. In this research, genistin was obtained by extracting from soybean meal powder, and then by adding polycaprolactone (PCL), genistin nanocapsules were prepared. For the first time, we used a lipophilic nanophase (encapsulated genistin) coated in a hydrophilic nanophase (gelatin /polyvinyl alcohol) as a dual nanosystem by the electrospinning method. In the approach, the nanofibers mimic the natural extracellular matrix, interact favorably with cells being cultured from one side, and raise the local concentration of a bioactive compound at the cell surface. The encapsulated drug which was inserted in fibers with a loading percentage of 92.01% showed appropriate and significant controlled release using high-performance liquid chromatography (HPLC). To prove the experiments, analysis using an ultraviolet–visible spectrometer (UV–Vis), 1H NMR spectrometer, Fourier transforms infrared spectrometer (FTIR), mechanical test, scanning electron microscope (SEM) and microscope transmission electron microscopy (TEM) was performed. The sample synthesized with 40% drug using the MTT method exhibited remarkable biological effects, viability, and non-toxicity. Additionally, significant proliferation and adhesion on the mouse fibroblast cell line L929 were observed within a 72-h timeframe. [ABSTRACT FROM AUTHOR]

The HYPNOESYS method (Hyperpolarized NOE System), which relies on the dissolution of optically polarized crystals, has recently emerged as a promising approach to enhance the sensitivity of NMR spectroscopy in the solution state. However, HYPNOESYS is a single‐shot method that is not generally compatible with multidimensional NMR. Here we show that 2D NMR spectra can be obtained from HYPNOESYS‐polarized samples, using single‐scan acquisition methods. The approach is illustrated with a mixture of terpene molecules and a benchtop NMR spectrometer, paving the way to a sensitive, information‐rich and affordable analytical method. [ABSTRACT FROM AUTHOR]

Enhancing magnetic resonance signal via hyperpolarization techniques enables the real‐time detection of metabolic transformations even in vivo. The use of para‐hydrogen to enhance 13C‐enriched metabolites has opened a rapid pathway for the production of hyperpolarized metabolites, which usually requires specialized equipment. Metabolite precursors that can be hyperpolarized and converted into metabolites at any given field would open up opportunities for many labs to make use of this technology because already existing hardware could be used. We report here on the complete synthesis and hyperpolarization of suitable precursor molecules of the side‐arm hydrogenation approach. The better accessibility to such side‐arms promises that the para‐hydrogen approach can be implemented in every lab with existing two channel NMR spectrometers for 1H and 13C independent of the magnetic field. [ABSTRACT FROM AUTHOR]

Stomata are the gatekeepers of plant water use and must quickly respond to changes in plant water status to ensure plant survival under fluctuating environmental conditions. The mechanism for their closure is highly sensitive to disturbances in leaf water status, which makes isolating their response to declining water content difficult to characterise and to compare responses among species. Using a small‐scale non‐destructive nuclear magnetic resonance spectrometer as a leaf water content sensor, we measure the stomatal response to rapid induction of water deficit in the leaves of nine species of eucalypt from contrasting climates. We found a strong linear correlation between relative water content at 50% stomatal conductance (RWCgs50) and mean annual temperature at the climate of origin of each species. We also show evidence for stomata to maintain control over water loss well below turgor loss point in species adapted to warmer climates and secondary increases in stomatal conductance despite declining water content. We propose that RWCgs50 is a promising trait to guide future investigations comparing stomatal responses to water deficit. It may provide a useful phenotyping trait to delineate tolerance and adaption to hot temperatures and high leaf‐to‐air vapour pressure deficits. SUMMARY STATEMENT: Nine species of eucalypt from contrasting climates and grown in a common climate (Angophora crassifolia, Corymbia tessellaris, Eucalyptus atrata, Eucalyptus caesia, Eucalyptus grandis, Eucalyptus laevopinea, Eucalyptus longifolia, Eucalyptus macrandra and Eucalyptus tereticornis) demonstrated a strong linear correlation between relative water content at 50% stomatal conductance (RWCgs50) and mean annual temperature at the climate of origin. [ABSTRACT FROM AUTHOR]

The field of zero- to ultralow-field (ZULF) nuclear magnetic resonance (NMR) is currently experiencing rapid growth, owing to progress in optical magnetometry and attractive features of ZULF-NMR such as low hardware cost and excellent spectral resolution achieved under ZULF conditions. In this work, an approach is proposed and demonstrated for simultaneous acquisition of ZULF-NMR spectra of individual 13C-containing isotopomers of chemical compounds in a complex mixture. The method makes use of fast field cycling such that the spin evolution takes place under ZULF conditions, whereas signal detection is performed in a high-field NMR spectrometer. This method has excellent sensitivity, also allowing easy assignment of ZULF-NMR spectra to specific analytes in the mixture. We demonstrate that the spectral information is the same as that given by ZULF-NMR, which makes the method suitable for creating a library of ZULF-NMR spectra of various compounds and their isotopomers. The results of the field-cycling experiments can be presented in a convenient way as 2D-NMR spectra with the direct dimension giving the high-field 13C-NMR spectrum (carrying the chemical-shift information) and the indirect dimension giving the ZULF-NMR spectrum (containing information about proton–carbon J-couplings). Hence, the method can be seen as a variant of heteronuclear J-resolved spectroscopy, one of the first 2D-NMR techniques. [ABSTRACT FROM AUTHOR]

REBa2Cu3Ox (REBCO) coated conductors are an enabling technology for >1 GHz nuclear magnetic resonance spectrometers that need >23.5 T solenoids, compact high-field fusion reactors beyond the International Thermonuclear Experimental Reactor, and 20 T class accelerator magnets. An in-depth understanding of stress and strain management is critically needed for these applications. Here, we report experimental data and an analysis of damages of REBCO-coated conductors in several scenarios relevant for their applications in high-field magnets and unique to their multi-layer thin film structure. The examined scenarios include failure induced by quench, failure induced by epoxy impregnation, and failure induced by a combination of epoxy impregnation and quench. The root cause is film blistering and peeling induced by thermally interfacial stresses characteristic of multilayered heteroepitaxial thin film structures on thick substrates utilized. The quantitative stress analysis is introduced using simple and easy to use formulas and clearly indicates how materials and structural characteristics affect the magnitude and the distribution of stresses and deflections. Finally, a simple method is introduced for removing degradation of REBCO coated conductors due to epoxy impregnation. Our data and analysis help our understanding of the practical limit of REBCO-coated conductors and can be utilized as a guidance for the physical design of REBCO coated conductors and high-current cables assembled from them and for minimizing damages. [ABSTRACT FROM AUTHOR]

This study introduces a low-field NMR spectrometer (LF-NMR) featuring a multilayer Halbach magnet supported by a combined mechanical and electrical shimming system. This setup offers improved field homogeneity and sensitivity compared to spectrometers relying on typical Halbach and dipole magnets. The multilayer Halbach magnet was designed and assembled using three nested cylindrical magnets, with an additional inner Halbach layer that can be rotated for mechanical shimming. The coils and shim-kernel of the electrical shimming system were constructed and coated with layers of zirconia, thermal epoxy, and silver-paste resin to facilitate passive heat dissipation and ensure mechanical and thermal stability. Furthermore, the 7-channel shim coils were divided into two parts connected in parallel, resulting in a reduction of joule heating temperatures from 96.2 to 32.6 °C. Without the shimming system, the Halbach magnet exhibits a field inhomogeneity of approximately 140 ppm over the sample volume. The probehead was designed to incorporate a solenoidal mini coil, integrated into a single planar board. This design choice aimed to enhance sensitivity, minimize B 1 inhomogeneity, and reduce impedance discrepancies, transmission loss, and signal reflections. Consequently, the resulting linewidth of water within a 3 mm length and 2.4 mm inner diameter sample volume was 4.5 Hz. To demonstrate the effectiveness of spectral editing in LF-NMR applications at 29.934 MHz, we selectively excited hydroxyl and/or methyl protons in neat acetic acid using optimal control pulses calculated through the Krotov algorithm. [ABSTRACT FROM AUTHOR]

HRMS-ESI: I m i / I z i [M + H] SP + sp calcd for C SB 11 sb H SB 7 sb Cl SB 2 sb N SB 2 sb O SB 3 sb : 284.9834; found: 284.9835. I Due to long relaxation time of the hydroxypyrimidine ring (when R SP 1 sp /R SP 3 sp = Me or R SP 1 sp /R SP 3 sp = H), some quaternary carbon signals may be broadened or even may not be responsive in SP 13 sp C NMR analysis. Keywords: isoxazoles; N-O bond cleavage; hydroxypyrimidines; molybdenum; one-pot; -amino enones; 1,3-diketones EN isoxazoles N-O bond cleavage hydroxypyrimidines molybdenum one-pot -amino enones 1,3-diketones 3841 3850 10 11/01/23 20231116 NES 231116 Graph Nitrogen-based heterocycles are one of the privileged core structural motifs in organic chemistry. HRMS-ESI: I m i / I z i [M + H] SP + sp calcd for C SB 10 sb H SB 6 sb ClF SB 3 sb N SB 3 sb O: 276.0151; found: 276.0157. [Extracted from the article]

Fragment‐based drug design is a well‐established strategy for rational drug design, with nuclear magnetic resonance (NMR) on high‐field spectrometers as the method of reference for screening and hit validation. However, high‐field NMR spectrometers are not only expensive, but require specialized maintenance, dedicated space, and depend on liquid helium cooling which became critical over the recurring global helium shortages. We propose an alternative to high‐field NMR screening by applying the recently developed approach of fragment screening by photoinduced hyperpolarized NMR on a cryogen‐free 80 MHz benchtop NMR spectrometer yielding signal enhancements of up to three orders in magnitude. It is demonstrated that it is possible to discover new hits and kick‐off drug design using a benchtop NMR spectrometer at low micromolar concentrations of both protein and ligand. The approach presented performs at higher speed than state‐of‐the‐art high‐field NMR approaches while exhibiting a limit of detection in the nanomolar range. Photoinduced hyperpolarization is known to be inexpensive and simple to be implemented, which aligns greatly with the philosophy of benchtop NMR spectrometers. These findings open the way for the use of benchtop NMR in near‐physiological conditions for drug design and further life science applications. [ABSTRACT FROM AUTHOR]

The article focuses on the development of a three dimensional (3D) printed quasi-optical sample holder to enhance the signal-to-noise ratio (SNR) in high-field electron paramagnetic resonance (HFEPR) spectrometers. Topics include the challenges of high-frequency electron paramagnetic resonance (EPR), the design and features of the quasi-optical sample holder, and its applications in different EPR modes.

Pyrolysis bio‐oils, one of the products of lignocellulosic biomass pyrolysis, have the potential to be widely used as fuels. The chemical composition of bio‐oils is very complicated as they contain hundreds, if not thousands, of different, mostly oxygen‐containing, compounds with a wide distribution of physical properties, chemical structures, and concentrations. Detailed knowledge of bio‐oil composition is crucial for optimizing both the pyrolysis processes and for any subsequent upgrading into a more viable fuel resource. Here we report the successful use of low‐field, or benchtop, nuclear magnetic resonance (NMR) spectrometers in the analysis of pyrolysis oils. Pyrolysis oils from four different feedstocks were derivatized and analyzed using 19F NMR techniques. The NMR results compare favorably with titrations for total carbonyl content. In addition, the benchtop NMR spectrometer proves able to reveal key spectral features, thus allowing the quantification of different carbonyl groups, such as aldehydes, ketones and quinones. Benchtop NMR spectrometers are typically compact, cheaper than their superconducting counterparts and do not require cryogens. Their use will make NMR analysis of pyrolysis oils easier and more accessible to a wide range of different potential users. [ABSTRACT FROM AUTHOR]

The mixture was quenched with H SB 2 sb O (20 mL) and CH SB 2 sb Cl SB 2 sb (100 mL) was added. The reaction mixture was then stirred for 12 h at rt, quenched with H SB 2 sb O (10 mL), and CH SB 2 sb Cl SB 2 sb (75 mL) was added. Keywords: phosphines; aryl chloride; chelating ligands EN phosphines aryl chloride chelating ligands 2737 2741 5 08/17/23 20230901 NES 230901 Graph Phosphines represent the most widely used ligand class in homogeneous catalysis. [Extracted from the article]

High‐temperature superconducting (HTS) materials have recently been incorporated into the construction of HTS cryogen‐free magnets for nuclear magnetic resonance (NMR) spectroscopy. These HTS NMR spectrometers do not require liquid cryogens, thereby providing significant cost savings and facilitating easy integration into chemistry laboratories. However, the optimal performance of these HTS magnets against standard cryogen NMR magnets must be evaluated, especially with demanding modern NMR applications such as NMR in anisotropic media. The stability of the HTS magnets over time and their performance with complex pulse sequence experiments are the main unknown factors of this new technology. In this study, we evaluate the utility of our prototype 400 MHz cryogen‐free power‐driven HTS NMR spectrometer, installed in the fumehood of a chemistry laboratory, for stereochemical analysis of three commercial natural products (artemisinin, artemether, and dihydroartemisinin) via measurement of anisotropic NMR data, in particular, residual dipolar couplings. The accuracy of measurement of the anisotropic NMR data with the HTS magnet spectrometer is evaluated through the CASE‐3D fitting protocol, as implemented in the Mestrenova‐StereoFitter software program. [ABSTRACT FROM AUTHOR]

Nuclear magnetic resonance (NMR) relaxometry is an analytical method that provides information about molecular environments, even for NMR "silent" molecules (spin-0), by analyzing the properties of NMR signals versus the magnitude of the longitudinal field. Conventionally, this technique is performed at fields much higher than Earth's magnetic field, but our work focuses on NMR relaxometry at zero and ultra-low magnetic fields (ZULFs). Operating under such conditions allows us to investigate slow (bio)chemical processes occurring on a timescale from milliseconds to seconds, which coincide with spin evolution. ZULFs also minimize T2 line broadening in heterogeneous samples resulting from magnetic susceptibility. Here, we use ZULF NMR relaxometry to analyze (bio)chemical compounds containing 1H-13C, 1H-15N, and 1H-31P spin pairs. We also detected high-quality ULF NMR spectra of human whole-blood at 0.8 μT, despite a shortening of spin relaxation by blood proteomes (e.g., hemoglobin). Information on proton relaxation times of blood, a potential early biomarker of inflammation, can be acquired in under a minute using inexpensive, portable/small-size NMR spectrometers based on atomic magnetometers. NMR relaxometry can provide information on paramagnetic as well as diamagnetic compounds in solution by analyzing nuclear-spin relaxation times, and, operated at ultra-low magnetic fields, slow processes can be studied. Here, the authors employ zero and ultra-low magnetic fields using an atomic magnetometer as a simple, portable, robust, inexpensive, and sensitive tool to analyze chemical solutions and biofluids. [ABSTRACT FROM AUTHOR]

Amino acids (AAs) and ammonia are metabolic markers essential for nitrogen metabolism and cell regulation in both plants and humans. NMR provides interesting opportunities to investigate these metabolic pathways, yet lacks sensitivity, especially in case of 15N. In this study, spin order embedded in p‐H2 is used to produce on‐demand reversible hyperpolarization in 15N of pristine alanine and ammonia under ambient protic conditions directly in the NMR spectrometer. This is made possible by designing a mixed‐ligand Ir‐catalyst, selectively ligating the amino group of AA by exploiting ammonia as a strongly competitive co‐ligand and preventing deactivation of Ir by bidentate ligation of AA. The stereoisomerism of the catalyst complexes is determined by hydride fingerprinting using 1H/D scrambling of the associated N‐functional groups on the catalyst (i.e., isotopological fingerprinting), and unravelled by 2D‐ZQ‐NMR. Monitoring the transfer of spin order from p‐H2 to 15N nuclei of ligated and free alanine and ammonia targets using SABRE‐INEPT with variable exchange delays pinpoints the monodentate elucidated catalyst complexes to be most SABRE active. Also RF‐spin locking (SABRE‐SLIC) enables transfer of hyperpolarization to 15N. The presented high‐field approach can be a valuable alternative to SABRE‐SHEATH techniques since the obtained catalytic insights (stereochemistry and kinetics) will remain valid at ultra‐low magnetic fields. [ABSTRACT FROM AUTHOR]